糠醛合成1,2-二乙酰氧基-1,2-双(2-呋喃基)乙烯的新工艺

A New Technology of Synthesizing 1,2-Diacetoxy-1,2-di-2- furanyl-ethylene with Furfural

以糠醛为原料 ,VB1 为催化剂 ,利用偶姻缩合合成了糠偶姻 ,并以此为原料 ,改变以往先溶解后降温 ,然后在低温下反应的传统工艺 ,使其醋酸酐化得到 1,2 二乙酰氧基 1,2 双 ( 2 呋喃基 )乙烯。讨论了反应温度、反应时间、催化剂用量以及投料比等因素对产物收率的影响 ,确定最佳合成工艺条件为 :反应温度 130～ 140℃ ,反应时间 3h ,催化剂、糠偶姻与醋酸酐的物质的量比为 0 0 2 88∶0 0 15 6∶0 0 85 3。产物的收率提高到 86 1% ,其熔点为 2 0 2～ 2 0 4℃。通过元素分析、GC -Mass谱、IR谱、1 HNMR谱对所合成的化合物进行了全面分析表征 。

Furoin was synthesized by acyloin condensation starting from furfural and VB\-1 as a catalyst.1,2Diacetoxy1,2di2furanylethylene was synthesized by furoin with a new technology which was different from the traditional one in that all of the reactants was dissolved before the reaction was carried out at low temperature.Factors affecting the yield of the products were discussed,such as reaction temperature,reaction time,the quantity of catalyst and the ratio of furoin to acetic anhydride.The optimum reaction conditions were as follows:reaction temperature 130-140 ℃,reaction time 3 h,the molar ratio of catalyst to furoin to acetic anhydride 00288∶00156∶0.0853.Under these conditions,the yield of the products was raised from 20%(or an unknown yield) to 86.1%,the m.p. of the product was 202-204 ℃.By characterization with elementary analysis,GC-Mass spectrum,IR spectrum and 1 HNMR,the structural formula of 1,2diacetoxy1,2di2furanylethylene was demonstrated.