HRID2353986

反应详情

EQUATION

反应方程式

HRID 2353986 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

A mixture of 5-[Acetyl-(3,5-bis-trifluoromethyl-benzyl)-amino]-8-chloro-2,3,4,5-tetrahydro-benzo[b]azepine-1-carbonyl chloride (1.0 mmol, 0.52 g) and hydrazine hydrate (50.0 mmol, 1.56 mL) in MeOH (5 mL) was refluxed at 70° C. for 12 h with vigorous stirring. The solvent was removed in vacuo and the crude product was purified by crystallization using EtOAc. The product was obtained as white solid; Rf 0.2 (EtOAc); MS (ES+): 523 (M+H+).

WORKUP

后处理

  1. customThe solvent was removed in vacuo
  2. customthe crude product was purified by crystallization
  3. customThe product was obtained as white solid