PENUNTUN PRAKTIKUM SINTESIS OBAT PENYUSUN : Drs. Nahitma Ginting M.Si., Apt. Prof. Dr. Ginda Haro M.Sc., Apt. Dra. Masria Lasma Tambunan, M.Si., Apt. Henny Sri Wahyuni S.Farm.,M.Si., Apt. LABORATORIUM KIMIA ORGANIK FAKULTAS FARMASI UNIVERSITAS SUMATERA UTARA MEDAN 2019 LABORATORIUM KIMIA ORGANIK PENUNTUN PRAKTIKUM SINTESIS OBAT Drs. Nahitma Ginting M.Si., Apt Prof. Dr. Ginda Haro M.Sc., Apt Dra. Masria Lasma Tambunan, M.Si., Apt. Henny Sri Wahyuni S.Farm.,M.Si., Apt Laboratorium kimia organik FAKULTAS FARMASI UNIVERSITAS SUMATERA UTARA Penuntun Praktikum Sintesis Obat LABORAN: NURLAILI, S.Si ASISTEN: CHRISTINA YANTI SIBURIAN S.Farm DATITHARINA Br.BARUS S.Farm FRANSISCA ARVIANTY TARIGAN S.Farm PANI REFLESIA NAINGGOLAN S.Farm EKO KESATRIA SURBAKTI EVI JULIANI DAMANIK IAS ZILENA KEZIA ARYANI BUKIT LEA AMANDA GINTING Laboratorium Kimia Organik Fakultas Farmasi Universitas Sumatera Utara Medan TATA TERTIB LABORATORIUM 1. Di dalam laboratorium, kebersihan, kerapian, kecakapan, ketelitian, dan ketertiban sangat penting. Semuanya akan menentukan nilai praktikum. 2. Harus memakai jas laboratorium lengan panjang, masker, sarung tangan, tanda pengenal dan sepatu tertutup sewaktu melaksanakan praktikum. 3. Dilarang makan, minum, merokok, memakai jam tangan, cincin, softlens dan telepon seluler sewaktu melaksanakan praktikum. 4. Setiap percobaan dan tugas-tugas, harus dikerjakan dengan baik bersama dengan partner kecuali yang bersifat perorangan. 5. Jika ragu-ragu tentang cara mengerjakan atau maksud praktikum hubungi staf atau asisten yang bertugas. 6. Menguasai materi yang dicobakan. 7. Menyerahkan jurnal resmi selambat-lambatnya seminggu setelah percobaan selesai. 8. Mengembalikan alat percobaan sementara setelah praktikum selesai. 9. Mengembalikan alat atau meja selambat-lambatnya seminggu setelah semua percobaan selesai. 10. Jika berhalangan praktikum, dilaporkan kepada staf atau asisten dengan membawa surat-surat yang diperlukan (surat dokter atau surat keterangan lain). 11. Harus hadir 15 menit sebelum praktikum dimulai. 12. Setiap praktikan wajib mengikuti responsi. 13. Untuk melengkapi percobaan, maka setiap praktikan membuat laporan studi literatur dan masing-masing judul tidak boleh sama (studi literatur dibuat setelah menyelesaikan semua judul praktikum). 14. Bagi yang tidak mengindahkan tata tertib ini, maka semua percobaannya akan dibatalkan. Plt Kepala Laboratorium Kimia Organik Henny Sri Wahyuni, S.Farm, M.Si., Apt. NIP 198509222018032001 Percobaan 1 Sintesis Parasetamol Pembuatan Nitrobenzen Synthesis Of Paracetamol Making Nitrobenzene Objective To make nitrobenzene by using synthesis nitration process on electrophilic aromatic substitution of benzene. Teori Benzena dan beberapa radikal aromatis merupakan komponen dari metil benzoat, anilin, dan sulfa-sulfa. Dapat dinitrasi dengan campuran nitril dan asam sulfat yang mengalami ionisasi lengkap untuk menghasilkan ion nitronium dan ion hidronium. Dalam suasana panas, asam nitrat merupakan pereaksi oksidasi yang baik. Susunan aromatis yang aktip seperti amin dan fenol dapat dinitrasi hanya dengan menggunakan asam nitrat pekat. Kuatnya ring benzena yang tidak aktif, yang dapat ditemukan pada nitrobenzene dan dengan adanya asam sulfat pekat dan asam nitrat pekat untuk menghasilkan meta-dinitrobenzene. Kelompok nitro lebih mudah mereduksi menjadi amin, dengan adanya nitrogen dan katalis logam, besi, Zn dan lain-lain. Aromatisitas benzena menyajikan suatu kestabilan yang unik pada sistem phi dan benzena tidak mengalami kebanyakan reaksi yang khas pada alkena. Meskipun demikian, benzena tidaklah lamban reaksinya (inert). Pada kondisi yang tepat, benzena mudah bereaksi substitusi aromatik elektrofilik. Alat Pendingin bola Labu alas bulat Hot plate Magnetic stirrer Corong pisah Termometer Erlenmeyer Apparatus Ball condensor Round bottom flask Hot plate Magnetic Stirrer Separating funnel Thermometer Erlenmeyer Bahan Benzena HNO3 pekat H2S04 pekat Akuades Na2SO4 anhidrat Es batu Garam Materials Benzene Conc HNO3 Conc H2S04 Aquadest Na2SO4 anhydrate Ice cube Salt Prosedur Dimasukkan 20 ml HNO3 pekat ke dalam labu alas bulat dan ditambahkan 20 ml H2S04 pekat sedikit demi sedikit melalui dinding labu sambil dikocok. Jaga campuran ini tetap dingin. Dimasukkan 15 ml benzena secara perlahan-lahan melalui dinding labu, kocok kuat-kuat pada setiap penambahan supaya tercampur sempurna dan jaga suhu tidak lebih dari 55 °C. Dipasang pendingin bola dan direfluks pada suhu 55-60 °C selama 45 menit. Dituangkan cairan hasil refluks ke dalam corong pisah yang telah berisi akuades, digojok lalu didiamkan. Diambil lapisan atas dan dimasukkan ke dalam erlenmeyer. Ditambahkan Na2SO4 anhidrat secukupnya, dikocok lalu didiamkan selama ± 24 jam. Procedure Put 20 ml HNO3 into a round bottom flask and add 20 ml of conc H2S04 little by little through the walls of the flask while shaken . Keep this mixture cool. Put 15 ml of benzene slowly through the wall of the flask , shake vigorously on any additions that perfectly mixed and maintain temperature not more than 55 ° C . Set up the reflux apparatus. Reflux at the temperature of 55-60 ° C for 45 minutes . Poured liquid reflux results into separating funnel already containing distilled water , shake and then allowed to stand . The top layer is taken and put in erlenmeyer . Add Na2SO4 anhydrate sufficiently, shake and then allowed to stand for ± 24 hours . Stuktur Parasetamol: Gambar Rangkaian Alat Refluks: Air keluar Klem Kondensor Statif Air masuk Labu alas bulat Stirrer control Hot plate control Figure Apparatus of Reflux Water Out Clamp Condensor Stative Water in Round bottom flask Stirrer control Hot plate control Percobaan 2 Sintesis Parasetamol Pemurnian Nitrobenzen Synthesis Of Paracetamol Purification Nitrobenzene Objective To make nitrobenzene by using synthesis nitration process on electrophilic aromatic substitution of benzene. Teori Nitrobenzen merupakan cairan berwarna kuning pucat dan memiliki aroma seperti aroma benzaldehid. Tidak larut dalam air tetapi dapat bercampur dengan alkohol dan eter. Memiliki titik didih 210-211 °C dan berat molekul 123,1. Dalam 1 ml memiliki berat sekitar 1,203 gram. Alat Corong Kertas saring Labu alas bulat bercabang Termometer Pendingin udara Hot plate Statif dan klem Vial Apparatus: Funnel Filter paper Round bottom flask branched Thermometer Air condensor Hot plate The stative and clamp Vial Bahan Lapisan Nitrobenzen Minyak goreng Materials Layer of nitrobenzene Cooking oil Prosedur Disaring nitrobenzen yang telah didiamkan selama ± 24 jam (apabila nitrobenzen tidak jernih, panaskan di atas penangas air dan kocok sampai jernih dan dinginkan). Dimasukkan ke dalam labu alas bulat bercabang. Didestilasi pada suhu 206-211 °C. Diukur volume destilat dan dimasukkan ke dalam vial. Procedure Layer of nitrobenzene that allowed for ± 24 hours (if nitrobenzene NOT clear, heat in the waterbath and shake up clear and cooling downed) . Put into the round bottom flask branched Distille at temperature of 206 - 211°C . Measured volume of distillate and add into the vial Gambar Rangkaian Alat Termometer Gabus Labu alas bulat bercabang Pendingin udara Penangas Wadah destilat Hot plate Figure Apparatus Of Destilation Nitrobenzene Thermometer Cork Round bottom flask branched Air condensor Bath Erlenmeyer Hot plate Pertanyaan : 1. Apa yang dimaksud dengan : Sintesis Retrosintesis Elektrofilik Nukleofilik 2. Tuliskan mekanisme reaksi sintesis parasetamol! 3. Jelaskan fungsi penambahan setiap bahan! 4. Jelaskan dan gambarkan perbedaan antara pendingin bola dan pendingin udara! 5. Mengapa pada destilasi pemurnian nitrobenzen digunakan minyak goreng? Question : 1. What is the meaning of : Synthesis Retrosynthesis Electrophilic Nucleophilic 2. Write the reaction mechanism of the synthesis of paracetamol! 3. Describe the function of adding each material! 4. Describe and illustrate the difference between the air condensor and ball condensor! 5. Why does the distillation purification of nitrobenzene used cooking oil? 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Percobaan 3 Saponifikasi Pembuatan Sabun Saponification Making Soap Objective To make a soap and see the mechanism of saponification. Teori Lemak atau minyak adalah triester dari gliserol yang dinamakan trigliserida. Trigliserida sederhana terdapat di alam, umumnya terdiri dari campuran trigliserida. Beberapa minyak menghasilkan satu atau dua macam asam lemak. Misalnya minyak zaitun terdiri dari 82% asam oleat. Trigliserida terdiri dari lemak dan minyak yang dapat dihidrolisa dengan berbagai cara, yang paling umum adalah dengan alkali atau enzim lipase. Hidrolisis dengan alkali disebut penyabunan, karena salah satu hasilnya adalah garam asam lemak yang disebut sabun. Sabun adalah garam logam alkali dari asam-asam lemak. Sabun terutama mengandung garam C16 dan C18, juga beberapa karboksilat dengan bobot atom lebih rendah. Sabun dibuat dengan cara memanaskan lemak atau minyak dengan suatu basa dan terhidrolisa menjadi gliserol dan garam natrium atau kalium dari asam lemak. Sabun termasuk surfaktan, yaitu suatu senyawa yang dapat menurunkan tegangan permukaan. Surfaktan dikelompokkan atas: Surfaktan anionik Surfaktan kationik Surfaktan netral Yang tergantung pada sifat hidrofiliknya. Surfaktan menurunkan tegangan permukaan dengan cara mematahkan ikatan hidrogen pada permukaan. Alat Neraca Labu alas bulat Pendingin bola Termometer Penangas air Gelas Beker Apparatus Analytic balance Round bottom flask Ball condensor Thermometer Waterbath Beaker glass Bahan NaOH pellet Etanol Minyak goreng Material NaOH pellets Ethanol Cooking oil Prosedur Ditimbang sebanyak 20 gram NaOH pellet Dimasukkan ke dalam labu alas bulat Ditambahkan 75 ml etanol 96% Dikocok hingga larut Ditambahkan 80 gram minyak goreng Direfluks pada suhu 78 °C selama 30 menit Didestilasi pada suhu 78 °C Diambil residu Procedure Weighed 20 grams of NaOH pellets Put in a round bottom flask Add 75 ml of ethanol 96 % Shake until dissolved Add 80 grams of cooking oil Reflux at temperature of 78 ° C for 30 minutes Distilled at temperature of 78 ° C Taken residue Gambar rangkaian alat refluks: Air keluar Statif Kondensor Klem Air masuk Labu alas bulat Stirrer control Hot plate control Figure Apparatus of Reflux Water out Clamp Condensor Stative Water in Round bottom flask Stirrer control Hot plate control Percobaan 4 Saponifikasi Pencetakan Sabun Saponification Molding Soap Objective To make a soap and see the mechanism of saponification. Teori Pemanasan campuran menyebabkan air dan etanol akan menguap. Saat reaksi sempurna, maka gliserol perlu dipisahkan dari sabun. Hal ini dilakukan dengan menambahkan air ke campuran tersebut untuk membuatnya lebih berbentuk cair dan kemudian penambahan larutan jenuh dari air garam. Gliserol lebih mudah larut dalam air garam dibandingkan sabun, oleh sebab itu mengakibatkan pemisahan dari dua senyawa kimia ini. Proses ini disebut sebagai “salting out” sabun. Alat Penangas air Batang pengaduk Gelas Beker Cawan penguap Erlenmeyer Cetakan sabun Neraca Apparatus Waterbath Stirring rod Beaker glass Evaporator dish Erlenmeyer Soap mold Analytic balance Bahan Residu destilasi Akuades NaCl Parfum Pewarna Es batu Material Distillation residue Aquadest NaCl Perfume Dyes Ice cube Prosedur Ditambahkan 100 ml air panas ke dalam residu Diaduk Ditambahkan larutan NaCl jenuh lalu diaduk Didinginkan lalu diambil bagian padatan Dimasukkan ke dalam cawan penguap Diuapkan di atas waterbath hingga hampir kering Ditambahkan pewarna dan parfum Dicetak Ditimbang sabun yang terbentuk Dimasukkan ke dalam wadah Procedure Add 100 ml of hot water into the residue Stir Add a saturated NaCl solution and then stir Cooling down then taken part solids Put into a evaporator dish Evaporate on water bath until almost dry Add dyes and perfumes Put into soap mold Weighed soap formed Gambar sedian sabun yang telah dicetak: Pertanyaan : 1. Apa yang dimaksud dengan : Saponifikasi Salting out 2. Jelaskan mekanisme reaksi saponifikasi! 3. Tuliskan fungsi penambahan setiap bahan! 4. Jelaskan dan gambarkan mekanisme sabun membersihkan kotoran! 5. Jelaskan perbedaan sabun keras dan sabun lunak! Question : 1. What is the meaning of : Saponification Salting out 2. Describe the reaction mechanism saponification! 3. Write down the function of adding each materials! 4. Describe and illustrate the mechanism of soap to clean the dirt! 5. Explain the difference between hard soap and soft soap! 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Percobaan 5 Isolasi Minyak Atsiri Sokletasi Isolation Of Essential Oil Soxhlet Teori Minyak atsiri adalah minyak yang bersifat volatile yang mengandung persenyawaan ester yang bersifat non polar. Minyak atsiri secara umum terdapat pada tumbuh-tumbuhan. Dewasa ini penggunaan minyak atsiri sangat dibutuhkan sebagai pengharum, karminatif, dll. Pengambilan bahan yang mengandung minyak atsiri harus benar-benar diperhatikan, seperti waktu pengambilan, umur tumbuhan, bagian yang diambil, tempat tumbuh, dll. Umumnya minyak atsiri didapat dengan cara penyulingan, karena alasan murah dan praktis. Cara-cara mendapatkan minyak atsiri adalah: 1. Penyulingan Dengan air Dengan air dan uap Langsung dengan uap 2. Pemerasan 3. Ekstraksi Pelarut volatile Pelarut non volatile (enfleurage dan maserasi) Alat Penangas air Alat soklet Termometer Kertas saring Statif dan klem Labu alas bulat Gelas ukur Sirkulator Bunsen Apparatus Waterbath Soxhlet Apparatus Thermometer Filter paper The stative and clamp Round bottom flask Measuring cup Circulatory Bunsen Bahan Bunga cengkeh n-heksan Material Clove n-heksan Prosedur Ditimbang 30 gram serbuk cengkeh yang telah dihaluskan, lalu dibungkus dengan kertas saring Dimasukkan ke dalam tempat sampel di alat soklet Dirangkai alat soklet Ditambahkan pelarut n-heksan sebanyak 3 siklus (± 85 ml) melalui tempat sampel Diekstraksi dan dipertahankan suhunya 68,5 °C sampai warna pelarut tidak berwarna. Procedure Weighed 30 grams of powered cloves are mashed, then wrapped with filter paper Entered into the thimble (the sample is placed) at soxhlet apparatus Assembled the soxhlet apparatus Added the solvent (n-heksan) as much as 3 cycle (±85 ml) to the sample Extracted and maintened the temperature in 68.5 °C until color of solvent is colorless Gambar rangkaian alat : 1. Pelarut 2. Labu alas bulat 3. Vapor 4. Tempat sampel 5. Sampel 6. Batas atas sifon 7. Sifon 8. Penghubung 9. Kondensor 10. Air masuk 11. Air keluar Percobaan 6 Isolasi Minyak Atsiri Pemisahan Minyak Atsiri Isolation Of Essential Oil Separation Of Essential Oil Teori Minyak cengkeh dari bunga cengkeh yang dikeringkan dari tumbuhan Eugenia caryophyllata Thunberg. Mengandung tidak kurang dari 82% volume eugenol. Cairan tidak berwarna atau kuning pucat yang menjadi menghitam oleh waktu, dan memiliki aroma dan rasa dari cengkeh. Larut dalam 2 bagian alkohol 70%. Bersifat anestesi lokal pada sakit gigi, karminatif, germisida, dan zat pemberi rasa. Alat Labu alas bulat Pipa bengkok Pendingin liebig Termometer Erlenmeyer Pipa cabang tiga Gelas ukur Vial Apparatus Round bottom flask Crooked Pipe Liebig Condensor Thermometer Erlenmeyer Measuring cup Vial Bahan Hasil sokletasi bunga cengkeh Material Result of extraction from cloves by soxhlet method Prosedur Didestilasi hasil sokletasi bunga cengkeh pada suhu 50-52 °C Diukur volume minyak cengkeh Dimasukkan ke dalam vial Procedure Distilled the result of soxhlet at 50-52 °C Measured the volume of essential oils Entered it into the vial Pertanyaan : 1. Jelaskan cara mengisolasi minyak atsiri, keuntungan, dan kelemahannya! 2. Tuliskan komponen minyak atsiri dalam sampel! 3. Jelaskan prinsip alat soklet! 4. Apa yang dimaksud dengan 1 siklus? 5. Tuliskan minimal 5 tumbuhan penghasil minyak atsiri beserta kandungan dan rumus bangunnya! Questions : 1. Explain how to isolate the essential oils, the advantages and disadvantages of the method! 2. Write the essential oils components in the sample! 3. Explain about the principles of soxhletation! 4. What is meant “1 cycle” in soxhletation? 5. Write minimal 5 plants which produce the essential oils, write the components and the chemistry structure! 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Percobaan 7 Sintesis Metil Salisilat Pembuatan Metil Salisilat Synthetis Of Methyl Salycilate Making Of Methyl Salycilate Teori Metil salisilat pertama kali diisolasi pada tahun 1843 dengan ekstraksi dari tumbuhan wintergreen (Gaultehria). Kemudian dengan cepat ditemukan bahwa senyawa ini memiliki sifat analgesic dan antipiretik yang hampir sama dengan asam salisilat ketika dipakai secara internal. Sifat medis ini mungkin diturunkan ketika metil salisilat dihidrolisa menjadi asam salisilat pada pH basa di usus. Metil salisilat dibuat dengan menggunakan asam salisilat sebagai bahannya, yang diesterifikasi pada grup karboksilat dengan methanol, dimana esterifikasinya merupakan reaksi kesetimbangan dengan menggunakan katalis asam. Kesetimbangan tidak akan bergerak jauh ke kanan untuk membentuk ester dengan hasil tinggi. Produk dapat dihasilkan dengan konsentrasi lebih bila kita menambahkan salah satu pereaksinya. Dalam percobaan ini, penambahan metanol dalam jumlah besar akan menggeser kesetimbangan sepenuhnya ke arah pembentukan ester. Alat Labu alas bulat Magnetic stirrer Termometer 1100C Pendingin bola Corong pisah Erlenmeyer Gelas ukur Neraca Gelas Beker Statif dan klem Hot plate Sirkulator Apparatus Round bottom flask Magnetic stirrer Termometer 1100C Air condensor Separating funnel Erlenmeyer Measuring cup Analytic balance Beaker glass The stative and clamp Hot Plate Circulatory Bahan Metanol Asam salisilat H2SO4 (p) CHCl3 Aquadest NaHCO3 Na2SO4 anhidrat Material Methanol Salicylate acid Conc H2SO4 CHCl3 Aquadest NaHCO3 Na2SO4 anhydrate Prosedur Dimasukkan 14 gram asam salisilat ke dalam labu alas bulat, lalu ditambah 50 ml metanol, dikocok hingga larut Ditambah 10 ml asam sulfat pekat, secara perlahan-lahan melalui dinding labu, lalu dimasukkan magnetic bar ke dalamnya Direfluks pada suhu 68-700C selama 2 jam Dimasukkan larutan yang jernih ke dalam corong pisah yang telah berisi 25 ml aquadest dan 25 ml CHCl3 lalu dikocok Dibilas labu alas dengan 15 ml CHCl3 lalu dimasukkan ke dalam corong pisah, kemudian dikocok dan didiamkan Ditampung lapisan bawah dan dimasukkan ke dalam corong pisah yang berisi 25 ml NaHCO3 lalu dikocok dan didiamkan Ditampung lapisan bawah dalam Erlenmeyer Ditambahkan Na2SO4 anhidrat secukupnya Didiamkan selama 24 jam Procedure Added 14 grams of salicylic acid to the flask, then add 50ml of methanol, stir until dissolved Added 10 ml of sulfuric acid slowly from the wall of the flask, then entered the magnetic bar into the flask Refluxed at 68-70°C for 2 hours Entered the clear solution into the separating funnel which already containing the 25 ml of distilled water and 25 ml of CHCl3, then shake it. Rinsed the flask with 15 ml of CHCl3 then inserted into the separating funnel, shake it and wait until separate Accomodated the bottom layer and entered to the separating funnel which containing of 25 ml of NaHCO3 then shake it Accommodate the bottom layer to Erlenmeyer Added Na2SO4 anhidrat sufficiently Allowed to stanf for 24 hours Gambar rangkaian alat refluks: Air keluar Klem Kondensor Statif Air masuk Labu alas bulat Stirrer control Hot plate control Figure Apparatus of Reflux Water out Clamp Condensor Stative Water in Round bottom flask Stirrer control Hot plate control Percobaan 8 Sintesis Metil Salisilat Pemurnian Metil Salisilat Synthetis Of Methyl Salycilate Purification Of Methyl Salycilate Teori Percobaan ini menggunakan destilasi di bawah tekanan yang dikurangi untuk memurnikan cairan bertitik didih tinggi. Destilasi cairan bertitik didih tinggi pada tekanan atmosfer sering tidak memuaskan. Pada temperatur yang disyaratkan, material yang didestilasi (dalam kasus ini, ester) dapat terurai secara parsial atau bahkan terurai total dan menyebabkan kehilangan produk dan kontaminasi dari destilat. Ketika tekanan total dari dalam alat destilasi dikurangi maka titik didih dari senyawa dikurangi. Melalui cara ini senyawa dapat didestilasi tanpa terurai. Alat Labu alas Pipa bengkok Pendingin liebig Hot plate Erlenmeyer Vial Corong Apparatus Round bottom flask Liebig condensor Hot plate Erlenmeyer Vial Funnel Bahan Lapisan metil salisilat Material Layer of methyl salicylate Prosedur Disaring lapisan metil salisilat Dimasukkan filtrat ke dalam labu destilasi dan didestilasi pada suhu 61620C sampai semua klorofom habis menguap Diukur volume metil salisilat yang diperoleh Dimasukkan ke dalam via Procedure Filtered the methyl salicylate Entered into a distillation flask and distlled at temperature 61-62°C until all chloroform evaporated Measured the volume of methyl salicylate Entered into the vial Gambar rangkaian alat destilasi ; Pertanyaan : 1. Tuliskan mekanisme reaksi metil salisilat! 2. Tuliskan fungsi penambahan bahan! 3. Apa ciri khas metil salisilat? 4. Apa perbedaan sintesis aspirin dan metil salisilat? 5. Apa yang dimaksud dengan : Esterifikasi Interesterifikasi Transesterifikasi Questions : 1. Write the mechanism od methyl salisylate reaction! 2. Write the function of the addition of materials! 3. What is the caharteristic of methyl salicylate? 4. What is the different between aspirin and methy salicylate? 5. What is this meaning and tell when it used : Esterification Interesterification Transesterificatin Jawaban : 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Percobaan 9 Ekstraksi Kafein dari Daun Teh Pembuatan Kafein Extraction of Caffeine from Leave Tea Making Caffeine Teori Dalam percobaan ini, kafein diisolasi dari daun teh. Permasalahan utama dengan isolasi bahwa kafein tidak muncul sendiri dalam daun teh tetapi bersamasama oleh senyawa alamiah lain yang harus dipisahkan. Komponen utama dari daun teh adalah selulosa, yang merupakan struktur dasar dari semua sel tumbuhan. Selulosa merupakan senyawa yang tidak larut dalam air sehingga selulosa tidak memberi masalah. Kafein sebaliknya larut dalam air dan merupakan senyawa utam yang diekstraksi dalam larutan yang disebut teh. Tanin juga terlarut dalam air panas yang digunakan untuk mengekstraksi daun teh. Ketika tanin diekstraksi dalam air panas, tanin yang dapat terhidrolisa akan terhidrolisa secara parsial, yang berarti bahwa asam galat bebas juga terdapat dalam teh. Tanin karena merupakan kelompok fenol dan asam galat karena kelompok karboksilat sehingga keduanya bersifat asam. Jika kalsium karbonat ditambahkan, yang merupakan suatu basa maka akan terbentuk garam kalsium dari asam-asam ini. Kafein dapat dieksraksi dari larutan teh basa dengan metilen klorida, tetapi garam kalsium dari asam galat dan tanin tidak larut dalam metilen klorida dan tetap tertinggal sebagai padatan yang tidak larut. Alat Gelas beker Kertas saring Corong Corong pisah Penangas air Cawan penguap Erlenmeyer Apparatus Beaker glass Filtering paper Funnel Separating funnel Water bath Evaporating dish Erlenmeyer Bahan Serbuk teh Aquadest CHCl3 Materials Tea leaves Aquadest CHCl3 Prosedur Ditimbang serbuk daun teh sebanyak 30 gram, baru dimasukkan dalam beaker glass. Ditambah 300 mL aquadest dan 15 gram CaCO3 dipanaskan dan dibiarkan mendidih selama 20 menit Disaring larutan teh panas melalui corong dengan kertas saring dalam Erlenmeyer Ampas ditambah 50 mL aquadest dan didihkan selama ± 10 menit sambil diaduk Disaring larutan teh panas dan dicampur dengan larutan teh yang pertama dan didinginkan Dipindahkan larutan teh kedalam corong pisah Diekstraksi sebanyak 4 kali masing-masing dengan 25 mL CHCl3 dan diambil lapisan bawahnya Didestilasi larutan Dimasukkan kedalam cawan penguap Diuapkan pelarut kloroform diatas penangas air hingga kering Procedure Weight tea leaves powder 30 g, and then put into beaker glass. Add 300 ml aquadest and 15 g CaCO3, heat and let it boiled for 20 minutes. Filter the hot tea solution use funnel with filtering paper into Erlenmeyer flask. The Residue add aquadest 50 ml and stir until boiling for ±10 minutes. Filter the hot tea solution and add to the first tea solution and cooling down. Move the tea solution in to separating funnel Extraction for 4 times with CHCl3 25 ml and take under layer Distilation the solution Put into evaporating dish Evaporate chloroform solution on the water bath until dry. Gambar rangkaian alat destilasi : Percobaan 10 Ekstraksi Kafein dari Daun Teh Pemurnian Kafein Extraction of Caffeine from Leave Tea Purification Caffeine Teori Kafein dapat dimurnikan dengan sublimasi. Kemudian ditutup, ketika kondisi vakum telah diperoleh baik, panaskan sampel perlahan dan hati-hati dengan micro burner untuk mensublimasi kafein. Pegang pembakar dan gerakkan api mundur dan maju di luar tabung uji. Jika sampel mulai meleleh, pindahkan api untuk beberapa detik sebelum dipanaskan lagi. Ketika sublimasi sempurna, pindahkan pembakar dan biarkan alat-alatnya mendingin. Alat Cawan penguap Kaca arloji Bunsen Apparatus Evaporating dish Watch glass Bunsen Bahan Kafein crude Materials Caffeine crude Prosedur Diletakkan gelas arloji di atas cawan lalu diletakkan kapas yang telah dibasahi dengan air diatasnya dimurnikan kafein crude dengan cara sublimasi Dipanaskan dengan menggunakan api kecil hingga tersublimasi sempurna) Ditimbang berat kafein murni Dimasukkan ke dalam pot plastik Dihitung persentase kafein murni kafein terhadap kafein crude Dihitung persentase kafein terhadap berat daun teh mula-mula Procedure Place a watch glass over the evaporating dish and then put cotton wetted with water on top. Purified caffeine crude with sublimation. Heated use low flame until sublimation perfect. Weight caffeine crude Calculated the percentage of pure caffeine to caffeine crude Calculated the percentage of caffeine to weight of tea leaves early. Pertanyaan : 1. Sebutkan kandungan daun teh beserta kelarutannya! 2. Senyawa apa saja yang mungkin ada dalam ekstraksi kafein yang pertama dengan air panas? 3. Berapa titik leleh dari kafein? 4. Sebutkan tumbuhan beserta famili, yang memiliki kandungan kafein! 5. Sebutkan dan jelaskan cara memurnikan kafein (min 2)! Question : 1. Identify content of the tea leaves and its solubility! 2. What is any compounds that may be present in the first caffeine extraction with hot water? 3. How many degrees melting point of caffeine? 4. Identify plants and their family who have compound of caffeine! 5. Identify and explain how to purify the caffeine! 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Percobaan 11 Pembuatan Saccharas Ferricus Production Saccharas Ferricus Teori Besi untuk pemberian oral tersedia dalam bentuk berbagai garam dari sulfat, fumarat, glukonat, suksinat, glutamate dan laktas. Tidak ada perbedaan absorpsi diantara garam-garam Fe ini, jika ada mungkin disebabkan oleh perbedaan kelarutannya dalam asam lambung. SF (sakaras ferikus) diindikasikan untuk anemia berat dengan berbagai range dosis, diindikasikan untuk kurang darah, lesu, cepat lelah, kurang nafsu makan setelah melahirkan. Alat Botol timbang Cawan porselen Beaker gelas Neraca Kertas lakmus Lumpang dan alu Apparatus Weighing bottle Porcelen dish Beaker glass Analytic balance Litmus paper Mortar and pestle Bahan FeCl3 Air suling Na2CO3 Materials FeCl3 Distilled water Na2CO3 Prosedur 7,5 gram kristal FeCl3 dilarutkan dalam 75 mL air suling (larutan A) 13 gram natrium karbonat digerus dalam lumpang dengan penambahan air suling sedikit demi sedikit dan bagian jernih dituang, lakukan berulang-ulang sampai seluruh natrium karbonat larut (larutan B) Larutan B ditambahkan ke larutan A secara perlahan-lahan melalui dinding beaker glass dengan menggunakan batang pengaduk, dan akan terbentuk endapan berwarna coklat. Cuci endapan berulang-ulang dengan menggunakan air suling dengan cara menambahkan air ke dalamnya, kemudian didiamkan dan bagian cairan yang jernih dituang. 12 Percobaan Teori Pembuatan Saccharas Ferricus Lanjutan Production Saccharas Ferricus Continue Saccharas ferricus merupakan gula yang diperoleh dari glukosa dan fruktosa membentuk ikatan gula berupa disakarida dan mengandung logam besi (ferri) dalam suatu kompleks. Dimana gula besi (saccharas ferricus) ini merupakan suatu hasil dari reaksi suatu disakarida yaitu sukrosa dan garam besi. Alat Beaker glass Pipet tetes Cawan porselen Batang pengaduk Lumpang dan alu Timbangan Penangas air Apparatus Beaker glass Drop pipette Porcelen dish Stir bar Mortar and pestle Analytic balance Water bath Bahan NaOH Gula putih halus Larutan AgNO3 Materials NaOH Refined white sugar AgNO3 Solution Prosedur Cairan jernih diuji dengan penambahan argentum nitrat Tambahkan 25 mg gula dan 2-4 ml NaOH 4N Uapkan sampai kering di penangas air sambil diaduk Setelah kering, gerus homogen dan timbang beratnya Cukupkan beratnya sampai 100 gram dengan penambahan serbuk gula Procedure A clear part of liquid tested by addition of argentum nitrate Added 25mg sugar and 2-4ml NaOH 4 N Evaporated until dryness in a water bath while stirred After dry, crushed until homogenous and weight its weighing Added refined white sugar until its weight 100g. Pertanyaan : 1. Sebutkan semua pereaksi yang digunakan dan masing-masing kegunaannya! 2. Jelaskan dan gambarkan mekanisme ikatan antara Fe dengan haemoglobin darah! 3. Apa kegunaan dari saccharas ferricus? 4. Gambarkan ikatan antara gula disakarida dan ferri dalam saccharas ferricus! 5. Bagaimana mekanisme reaksi pembentukan saccharas ferricus? Questions : 1. Mention all of the reagents used and each purpose! 2. Describe and drawing the bond mechanism between Fe with blood hemoglobin! 3. What is the used of Saccharas ferricus! 4. Drawing the bond between disaccharide sugar and ferric in saccharas ferricus! 5. How is the reaction mechanism on formation of Saccharas ferricus? 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