HRID465647

反应详情

EQUATION

反应方程式

HRID 465647 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

A solution of (±)-N-[2,6-bis(1-Methylethyl)-phenyl]-2-bromopropanamide (2.0 g, 6.4 mmol), 2,2-diphenylethylamine (1.26 g, 6.41 mmol) and triethylamine (1.8 mL, 13 mmol) in acetonitrile (30 mL) was refluxed (96 hours), then cooled (25° C.). The resulting slurry was diluted with ethyl acetate (300 mL), washed with water (1×100 mL), with saturated aqueous sodium bicarbonate (1×100 mL), with brine (1×100 mL), then dried (MgSO4) and concentrated. Crystallization from ethyl acetate/hexane yielded 2.0 g (72.8%) of the title compound as a white solid, mp 206.5°-208.5° C.

WORKUP

后处理

  1. washwashed with water (1×100 mL), with saturated aqueous sodium bicarbonate (1×100 mL), with brine (1×100 mL)
  2. dry with materialdried (MgSO4)
  3. concentrationconcentrated
  4. customCrystallization from ethyl acetate/hexane