HRID1891018

反应详情

EQUATION

反应方程式

HRID 1891018 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of methyl 6-chloro-1H-indole-5-carboxylate (0.5 g, 2.4 mmol) in dichloromethane at 0 C, was added drop-wise, a solution of diethyl aluminum chloride (3.6 mL, 1M) and stirred under nitrogen for 45 min. To this mixture, added a solution of acetyl chloride (0.3 g, 3.8 mmol) in dichloromethane (3 mL). The resulting mixture was stirred for 3 h and at room temperature for 30 min. The reaction was quenched by the addition of cold Tris buffer (pH 7.5, 1 mM and added dichloromethane (2×15 mL). The solid that separated was removed by filtration, washed with water and dried to give the title compound (0.44 g, 73%), m/z=252 (M+H).

WORKUP

后处理

  1. customThe reaction was quenched by the addition of cold Tris buffer (pH 7.5, 1 mM
  2. additionadded dichloromethane (2×15 mL)
  3. customThe solid that separated
  4. customwas removed by filtration
  5. washwashed with water
  6. customdried