HRID1721480

反应详情

EQUATION

反应方程式

HRID 1721480 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Into 629 g of a toluene solution containing 144.7 g (0.462 mol, E/Z=25/75) of α-methoxyimino-2-(2,5-dimethylphenoxymethyl)phenylacetic acid produced in accordance with Example 5-(1) and 0.338 g (0.0046 mol) of dimethylformamide was introduced 68.5 g (0.692 mol) of phosgene over 10 hours while keeping at 60°-65° C., and the reaction was subsequently allowed to proceed at the same temperature for 2 hours and then at 80° C. for 2 hours. Then, excess phosgene was removed by distillation, followed by dilution with toluene, which afforded 612.6 g of a toluene solution of α-methoxyimino-2-(2,5-dimethylphenoxymethyl)phenylacetyl chloride.

WORKUP

后处理

  1. customwhile keeping at 60°-65° C.
  2. waitat 80° C. for 2 hours
  3. customThen, excess phosgene was removed by distillation