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微波辐照相转移催化合成苹果酯 被引量:7

Synthesis of Fructone under Microwave Irradiation and Phase Transfer Catalysis
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摘要 以乙酰乙酸乙酯和乙二醇为原料合成苹果酯。用单因素试验法和正交试验法探讨了催化剂、投料比、反应温度、反应时间和加热方式等因素对苹果酯合成的影响。试验结果表明 :在微波辐照下 ,最佳反应条件为 :以硫酸氢钠 /三氯化铁为催化剂、PEG -80 0为相转移催化剂、乙酰乙酸乙酯 :乙二醇 (mol)为 1 :1 .5~ 1 .8、甲苯为带水剂、微波功率为中低档、微波辐照时间为 8~ 1 2min ,产率可达 91 .5 %以上。产品经IR、1HNMR、MS和GC等测定 。 In this paper ethyl acetoacetate and ethanediol were used as raw material to synthesize fructone. By a single factor synthesis and an orthogonal test, the influences of catalysts, reactants ratio, temperature, time, heating ways and so on were studied. With microwave irradiation and phase transfer catalysts, the optimum reaction condition were as follows: NaHSO 4/FeCl 3 as catalyst, PEG-800 as phase transfer catalyst, ethyl acetoacetate: ethanediol was 1:1.5~1.8 (mol), methylbenzene as solvent, microwave irradiation time 8~12 min. The yield was up to 91.5%. The synthesis product was characterized by refraction index, chemical and physical property, IR, GC, MS and 1HNMR spectra.
出处 《香料香精化妆品》 CAS 2002年第5期18-21,共4页 Flavour Fragrance Cosmetics
关键词 微波辐照 相转移催化合成 苹果酯 相转移催化剂 Microwave irradiation Phase transfer catalyst Synthesis Fructone 1HNMR
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