HRID2307436

反应详情

EQUATION

反应方程式

HRID 2307436 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The solution of (S)-[1-(3-bromo-phenyl)ethyl]carbamic acid tert-butyl ester (2.6 g, 8.8 mmol), morpholin-2-yl-methanol (1.1 mg, 9.7 mmol), palladium acetate (10 mol %, 197 mg), 2-(di-t-butylphosphino) biphenyl (20 mol %, 523 mg), and sodium tert-butoxide (1.1 g, 1.3eq) in toluene (28 ml) was stirred in sealed tube at 80° C. for 4 days. The reaction mixture was filtered through Celite pad and washed with 10% methanol/dichloromethane. The filtrate was concentrated under vacuum and purified by flash chromatography with 40% acetone/hexane. Yellow solid was obtained as the title compound (1.0 g, 39% yield).

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered through Celite pad
  2. washwashed with 10% methanol/dichloromethane
  3. concentrationThe filtrate was concentrated under vacuum
  4. custompurified by flash chromatography with 40% acetone/hexane