HRID2053659

反应详情

EQUATION

反应方程式

HRID 2053659 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 169.9 kg of the dichloromethane solution of N-[(2-chlorophenyl)methyl]acetamide obtained in Example 3-(A), 47.1 kg (0.6 moles) of acetyl chloride was added and 108.0 kg (0.81 kmoles) of aluminum chloride was added at 15 to 30° C. over 1.5 hours. After dichloromethane was distilled off was distilled off under normal pressure until the temperature reaches 50° C. over 2 hours, the mixture was aged for 6 hours (objective product: other position isomers=76.75%:1.65%; GC area %). After the completion of the reaction, the resulting solution was added dropwise to 450 kg of water at 15 to 35° C. over 2 hours. The solution was extracted twice with 90 kg of dichloromethane and 40 kg of dichloromethane to obtain 199.8 kg of a dichloromethane solution of N-[(5-acetyl-2-chlorophenyl)methyl]acetamide.

WORKUP

后处理

  1. distillationAfter dichloromethane was distilled off
  2. distillationwas distilled off under normal pressure until the temperature
  3. waitthe mixture was aged for 6 hours
  4. customAfter the completion of the reaction
  5. extractionThe solution was extracted twice with 90 kg of dichloromethane and 40 kg of dichloromethane