微波辐射相转移催化合成苹果酯-B

采用微波辐射相转移催化技术,以四丁基溴化铵为相转移催化剂、乙酰乙酸乙酯和1,2-丙二醇为原料,柠檬酸为酸催化剂,在无有机溶剂存在下用单因素实验法和正交实验法研究了微波辐射功率、辐射时间、催化剂的类型和用量及反应物的摩尔比等因素对苹果酯-B收率的影响。实验结果表明,在微波辐射功率210W、辐射时间6m in、n(乙酰乙酸乙酯)∶n(1,2-丙二醇)=1.00∶2.00、n(柠檬酸)∶n(乙酰乙酸乙酯)=0.05的优化条件下,苹果酯-B的收率可达91.2%。

Synthesis of Eraistone -B Under Microwave Irradiation and on Phase Transfer Catalyst

Eraistone-B was synthesized from ethyl acetoacetate and 1,2-propanediol on phase transfer catalyst under microwave irradiation and without any organic solvent.By a single factor orthogonal test,effects of microwave power,irradiation time,catalysts,reactants ratio etc.on reaction were studied.Optimal reaction conditions were microwave power 210W,irradiation time 6min,n(ethyl acetoacetate) ∶n(1,2-propanediol)=1.00 ∶2.00,tetrabutyl ammonium bromide(TBAB)as phase transfer catalyst,citric acid as catalyst and n(citric acid) ∶n(ethyl acetoacetate)=0.05,yield of eraistone-B reached 91.2%.