HRID2054448

反应详情

EQUATION

反应方程式

HRID 2054448 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

Acetic anhydride (38.9 mL, 412 mmol) was added to a stirred solution of 3,4-dimethylaniline 1-5 (10.0 g, 82.5 mmol) in pyridine (150 mL) at ambient temperature. After stirring at approximately 60° C. for 2 h, the volatiles were removed in vacuo, and the residue was partitioned between diethyl ether and aqueous 1 N hydrochloric acid. The organic phase was separated and washed with saturated aqueous sodium bicarbonate, brine, dried (sodium sulfate) and concentrated in vacuo to afford 1-6 as a white crystalline solid.

WORKUP

后处理

  1. customthe volatiles were removed in vacuo
  2. customthe residue was partitioned between diethyl ether and aqueous 1 N hydrochloric acid
  3. customThe organic phase was separated
  4. washwashed with saturated aqueous sodium bicarbonate, brine
  5. dry with materialdried (sodium sulfate)
  6. concentrationconcentrated in vacuo