第 36 卷第 4 期 Vol. 36 No. 4 2006 年 8 月 Aug 2006

所属栏目：有机合成原料 2,3-二甲氧基-1,3-丁二烯的合成研究

王升文; 邓建成; 周广(湘潭大学化学学院; 湖南湘潭)

摘　要：选用新型催化剂及溶剂体系,通过相转移催化法在低温下合成了2,3-二甲氧基-1,3-丁二烯,采用减压蒸馏和柱层析的分离方法提高了产品纯度,通过在反应前引入吩噻嗪阻聚剂有效防止了产物聚合。实验表明:反应以十六烷基三甲基溴化铵作催化剂,v(2,3-丁二酮)∶v(原甲酸甲酯)=1∶3.5,并且在溶剂CH2Cl2中回流10h时,总收率达到77%。与文献相比,反应条件更温和,收率更高。

关键词：2; 3-二甲氧基-1; 3-丁二烯; 相转移催化; 合成

中图分类号：O621.3　　文献标识码：A　　文章编号：1009-9212(2006)04-0057-03

Synthesis of 2,3-Dimethoxy-1,3-butadiene

WANG Sheng-wen; DENG Jian-cheng; ZHOU Guang （Institute of Chemistry; Xiangtan University; Xiangtan 411105; China）

Abstract：2,3-dimethoxy-1,3-butadiene was synthesized under low temperature by phase transfer catalyst using new catalyst and solvent, the purity of product could be increased by combination of vaccum-distillation and column chromatography, polymerization of production could be prevented through the addition of phenothiasin before reaction. The experiment showed that the yield of reaction was the highest when cetrimonium bromide was taken as catalyst,the ratio(v : v) of 2,3-Butanedione and methyl o-formate was 1 : 3....

Key words：2; 3-dimethoxy-1; 3-butadiene; phase transfer catalyst; synthesis

收稿日期：2006-06-20

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