反应 #6549

反应方程式

phosgene

phosgene

phosgene

4-hydroxybenzophenone

→

4-chloroformylbenzophenone

收率 99.2%

溶剂

o-xylene

反应条件

后处理

1. 1
   温度During this time, the internal temperature was increased from 95° to 1200° C
2. 2
   其他The salt (catalyst) precipitated toward the end of the reaction
3. 3
   过滤was filtered off
4. 4
   workup.DISTILLATIONthe solvent was distilled off

实验过程

A total of 3.4 kg of phosgene were passed in the course of 5 hours into a solution of 4 kg of 4-hydroxybenzophenone and 190 g of benzyltrimethylammonium chloride in 11.4 kg of o-xylene. During this time, the internal temperature was increased from 95° to 1200° C. After the end of the introduction of phosgene, stirring was continued for 30 minutes at 115° C. Working up was carried out by expelling the excess phosgene with nitrogen. The salt (catalyst) precipitated toward the end of the reaction was filtered off and the solvent was distilled off. 4.9 kg (93%) of yellowish 4-chloroformylbenzophenone of melting point 67°-72° C. were obtained. This crude product containing 12.69% of Cl- (theoretical value 13.60%) was used directly for the subsequent reactions, without further purification.

来源