第 45 卷第 1 期Vol. 45 No. 1
2015 年 2 月Feb 2015

所属栏目:医药及中间体

无水丁二醛的制备方法
旷 东1,2,叶振君1,2,张洪玉1,2,毕 强1,董建生1,施顺发1,张芝平1* (1. 上海生农生化制品有限公司,上海 200231;2. 上海生华化学科技有限公司,上海 200231)
摘 要:以呋喃为原料,经溴化和甲氧基化得到2,5-二甲氧基二氢呋喃,再通过催化加氢合成得到2,5-二甲氧基四氢呋喃,进一步通过加热水解反应。减压蒸除反应溶剂,浓缩后得到丁二醛,含量98%(GC),3步反应总收率71%(以原料呋喃计)。反应条件温和,工艺简便,原料成本较低,有工业应用价值。
关键词:丁二醛;2,5-二甲氧基四氢呋喃;呋喃
中图分类号:TQ224.1  文献标识码:A  文章编号:1009-9212(2015)01-0033-03
Synthesis Method of Anhydrous Succinaldehyde
KUANG Dong1,2, YE Zhen-jun1,2, ZHANG Hong-yu1,2, BI Qiang1, DONG Jian-sheng1, SHI Shun-fa1, ZHANG Zhi-ping1* (1. Shanghai Shengnong Pesticide Co., Ltd., Shanghai 200231, China; 2. Shanghai Shenghua Chemical Technology Co., Ltd., Shanghai 200231, China)
Abstract:A synthetic method for the preparation of anhydrous succinaldehyde was developed. In this method, 2,5-dimethoxy-dihydrofuran was obtained via bromination and methoxylation reaction using furan as the starting material. Followed by catalytic hydrogenation of 2,5-dimethoxy-dihydrofuran, the key intermediate 2,5-dimethoxy-tetrahydrofuran was obtained. The pure final product was synthesized through hydrolysis reaction of 2,5-dimethoxy-tetrahydrofuran under heating condition. The purity of succinaldehyde was 98%, and the total yield of the three steps was 71%. This new process had the advantages of mild condition, simple process, and cheap materials.
Key words:succindialdehyde; 2,5-dimethoxy-dihydrofuran; furan
基金项目: “十二五”国家科技支撑计划项目资助(2011BAE06B01-16)。
作者简介:旷 东(1987-),男,重庆人,硕士,主要从事农药产品开发。
联 系 人:张芝平,教授级高级工程师,主要从事农用化学品的研制开发(E-mail:zhangzhiping05@sina.com)。
收稿日期:2014-11-25