SINTESIS FRUKTON DARI ETIL ASETOASETAT DAN ETILEN GLIKOL MENGGUNAKAN KATALIS ASAM FOSFOTUNGSTAT (H3PW12O40.H2O) - Kameliani Hibatulloh Gustiawan, - (2021)
Frukton merupakan bahan parfum dengan aroma buah apel dan dapat diperoleh melalui reaksi asetalisasi etil asetoasetat dan etilen glikol menggunakan katalis asam fosfotungstat (H3PW12O40.H2O). Penelitian ini bertujuan untuk mengetahui pengaruh metode refluks azeotrop menggunakan pelarut sikloheksana dan kondisi optimum dari pembentukan senyawa frukton menggunakan katalis asam fosfotungstat. Sintesis frukton dari etil asetoasetat dan etilen glikol menggunakan metode refluks azeotrop dilengkapi alat dean-stark dan pelarut sikloheksana. Penentuan kondisi optimum dilakukan menggunakan variasi suhu, rasio mol pereaksi, katalis, dan lama waktu reaksi. Variasi suhu reaksi dilakukan pada suhu 74°C, 75°C, 76°C, 78°C dan 81°C. Variasi mol pereaksi antara etil asetoasetat dan etilen glikol 1 : 1,5; 1: 2; dan 1 : 3. Variasi mol katalis asam fosfotungstat sebanyak 20 x 10-4 mol; 10 x 10-4 mol; 5 x 10-4 mol; 2,5 x 10-4 mol; dan 1,25 x 10-4 mol. Variasi waktu reaksi dilakukan pada 30 menit; 60 menit; 90 menit; 120 menit; 150 menit; 180 menit; 210 menit; dan 240 menit. Analisis hasil sintesis dilakukan menggunakan instrumen Kromatografi Gas (GC) dan Kromatografi Gas Spektrometri Massa (GC-MS). Ditemukan kondisi optimum sintesis frukton pada suhu 78°C, jumlah katalis 10 x 10-4 mol dengan rasio mol etil asetoasetat dan etilen glikol 1 : 3 selama 3 jam. Produk hasil reaksi diperoleh sebesar 93,42%. Fructone is a perfume ingredient with an apple aroma and can be obtained through the acetalization reaction of ethyl acetoacetate and ethylene glycol using a phosphotungstic acid (H3PW12O40.H2O) as a catalyst. This study aims to determine the effect of the azeotropic reflux method using cyclohexane as a organic solvent and the optimum conditions for the formation of fructone using phosphotungstic acid catalyst. Synthesis fructone from ethyl acetoacetate and ethylene glycol using cyclohexane-water azeotropic reflux method equipped with dean-stark apparatus. Determination of the optimum conditions was carried out using variations of temprature, mole ratio of the reagent, catalyst, and reaction time. Variation of temprature was carried out at 74°C, 75°C, 76°C, 78°C and 81°C. Variation of reagent mole between ethyl acetoacetate and ethylene glycol 1:1,5; 1:2; and 1: 3. Variation of moles of phosphotungstic acid catalyst as much as 20 x 10-4 mol; 10 x 10-4 mol; 5 x 10-4 mol; 2.5 x 10-4 mol; and 1.25 x 10-4 mol. Variation of reaction time was carried out at 30 minutes; 60 minutes; 90 minutes; 120 minutes; 150 minutes; 180 minutes; 210 minutes; and 240 minutes. Analysis of the synthesis results was carried out using Gas Chromatography (GC) and Gas Chromatography Mass Spectrometry (GC-MS) instruments. The optimum condition for fructone synthesis was found at a temperature of 78°C, the amount of phosphotungstic acid catalyst was 10 x 10-4 moles with a mole ratio of ethyl acetoacetate and ethylene glycol 1: 3 for 3 hours with the yield product obtained is 93,42%.