5-(2,3-二氯苯氧基)-4-氯-2-硝基苯胺合成工艺的研究

Synthesis conditions for 5-(2,3-dichlorophenoxy)-4-chloro-2-nitrobenzenamine

研究了以2,3-二氯苯酚和4,5-二氯-2-硝基苯胺通过缩合反应制备5-(2,3-二氯苯氧基)-4-氯-2-硝基苯胺的合成工艺。着重考察了催化剂、反应时间、加料速率、加料顺序等因素对缩合反应的影响。结果表明,不同催化剂对反应选择性的影响很大,采用适宜的催化剂可有效抑制副反应的发生,选择性可达95%。转化率随时间的延长而逐渐增加,反应选择性随时间的延长慢慢下降,反应时间宜控制在8 h左右,收率可达88%。

5 - （2,3 - dichlorophenoxy） - 4 - chloro - 2 - nitrobenzenamine, an important intermediate of triclabendazole was synthesized by using 2,3 - dichlorophenol and 4,5 - dichloro - 2 - nitrobenzenamine. Influences of catalysts, reaction time, the sequence and velocity of adding materials were observed. Selectivity was significant affected by the kind of catalysts. Selectivity was 95 % if the suitable catalyst was used. The conversion rate increased and selectivity decreased with time going on. Yield reached 88 % when reaction time was 8 hours and decreased after that. The by- reaction increased in alkaline environment.