HRID2230280

反应详情

EQUATION

反应方程式

HRID 2230280 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of the product from Example G (1.0 g, 2.18 mmol) was dissolved in DMF and cooled to 0° C. The resulting solution treated with NaH (2.18 mmol) and was stirred for 1 hour at 0° C. and treated with α-bromo-p-tolunitrile (0.45 g, 2.30 mmol). The reaction mixture was warmed to room temperature and stirred overnight. The reaction mixture was poured into a separatory funnel containing ethyl acetate (50 mL) and water (50 mL) and shaken. The organic phase was separated and washed with brine, dried, and concentrated to give the title compound (0.76 g, 61%).

WORKUP

后处理

  1. temperatureThe reaction mixture was warmed to room temperature
  2. stirringstirred overnight
  3. additionThe reaction mixture was poured into a separatory funnel
  4. stirringshaken
  5. customThe organic phase was separated
  6. washwashed with brine
  7. customdried
  8. concentrationconcentrated