摘要
由苯甲醛和丙酮酸为原料经缩合 ,还原 ,重排三步反应制得产品。用正交设计法对每一步反应的工艺条件进行优化 ,第一步缩合反应由文献值 66.7%提高到 79.9% ,得到最佳工艺为 :反应温度 0℃ ,反应时间为 1小时 ;第二步还原反应收率由文献值 3 2 %提高到82 % ,得到最佳工艺为 :水解温度 40℃ ,反应时间为 3小时 ,p H值为 1 ;第三步反应收率为3 2 %。全程收率为由文献值 1 1 %～ 1 5%提高到 2 1 %。在第二步制备 3 -苯甲叉乳酸时发现有二聚物产生。
The title compound has been prepared by three continuous reaction steps of condensation, reduction, rearrangement from benzaldehyde and pyruvic acid. The operation conditions were optimized by optimum seeking method. The results show that in the first step, the yield was raised to 79.9% comparing with the 66.7% in the literature, and the optimum conditions were as follows: condensation in the course of 1 hour and in 0℃. In the second step the yield reached 82% comparing with the 32% in the literature, and the optimum conditions were as follows: hydrolyzation in the course of 3 hours, in 40℃ and pH=1. And the yield was 32% in the third step. The overall yield reached as high as 21% comparing with 11%～15% in the literature. In the second step, it has been found that there was some dimer as byproduct besides the main product.
出处
《浙江工业大学学报》
CAS
2003年第1期78-81,共4页
Journal of Zhejiang University of Technology
基金
浙江省自然科学基金资助项目 (2 0 0 0 16 )
