HRID2118030

反应详情

EQUATION

反应方程式

HRID 2118030 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Acetyl chloride (0.1 ml, 1.4 mmol) was added to an ice cooled solution of the amine of example 4 (200 mg, 0.53 mmol) in dichloromethane (5 ml) and stirred at room temperature for 20 hours. Dichloromethane was evaporated off under reduced pressure and the residue purified by chromatography on silica gel using methanol in dichloromethane (5:95) as eluant. The residue was dissolved in dichloromethane (2 ml) and hydrochloric acid (1M in diethyl ether, 2 ml) was added, and the solvents evaporated under reduced pressure to give the title compound as a brown foam (110 mg).

WORKUP

后处理

  1. customDichloromethane was evaporated off under reduced pressure
  2. customthe residue purified by chromatography on silica gel
  3. dissolutionThe residue was dissolved in dichloromethane (2 ml)
  4. additionhydrochloric acid (1M in diethyl ether, 2 ml) was added
  5. customthe solvents evaporated under reduced pressure