摘要
报道了一种绿色合成胡椒烯丙酮 [31 6 0 - 37- 0 ]的新方法。这种不污染环境的合成方法是用洋茉莉醛 [1 2 0 - 57- 0 ]与丙酮 [6 7- 6 4 - 1 ]在水相和有机相之间进行克莱森 -施密特反应 ;产物分离后有机层循环再用 ,水层经过活性炭吸附处理后也循环使用 ,做到了无试验废水排放。 1mol洋茉莉醛、回收的苯溶液 2 0 0ml、补充丙酮 70ml、回收并且经过活性炭吸附处理后的水溶液 2 0 0ml、补充 1 .1g氢氧化钠 ,50℃反应 7h ,产率 99.7% ,纯度 99.6 %。
A 'green' method for the synthesis of 4-(1,3-benzediox ole)-3-buten-2-one is reported. which doesn't pollute environmen t.This method for synthesis of 4-(1,3-benze-dioxole)-3-buten-2-one uses Claison -Schmidt reaction of piperonal and acetone between wate r phase and organic phase.After the product was isolaed,the organic liquid can be used again,and after the water solution was absorbed by activated carbon,it can be used again,too.In the experiment,no waste waer was drained out.under the fol lowing conditions:piperonal 1.00mol,benzene liquid recovered 200ml,acetone added 70ml,water recovered and treated by activated carbon 200ml,NaOH added 1.1g,the reaction of them lasts for 7 hr at 50~{!f~},the yield rate reaches 99.7%,the purity of product is 99.6%.
基金
重庆市科委基金资助项目 (99- 5 85 6 )