巴氯芬的绿色制备工艺研究

Green Preparation of Baclofen

以对氯苯甲醛和丙二酸二甲酯为原料,经过Henry缩合、迈克尔加成、催化加氢以及脱羧4步反应制备得到巴氯芬,确定了催化加氢的优化条件为:以雷尼镍作为催化剂,用量为10%(m/m),反应温度为35℃,反应时间为6.5 h,套用次数不超过8次。优化条件下,中间体3收率95.5%,纯度98.5%。

Baclofen was prepared by Henry condensation,Michael addition, catalytic hydrogenation and decarboxylation with para-chlorobenzaldehyde and methylmalonate as raw materials. The reaction conditions were optimized as follows, Raney's Ni as catalyst, 10%(m/m), reaction temperature 35℃, reaction time 6.5 h, application number not more than 8 times, with intermediate 3 yield of 95.5% and purity of 98.5%.