HRID2118030
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customDichloromethane was evaporated off under reduced pressure
- customthe residue purified by chromatography on silica gel
- dissolutionThe residue was dissolved in dichloromethane (2 ml)
- additionhydrochloric acid (1M in diethyl ether, 2 ml) was added
- customthe solvents evaporated under reduced pressure