HRID603112

反应详情

EQUATION

反应方程式

HRID 603112 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-100 °C

PROCEDURE

实验过程

2-(4-bromophenyl)-2-methylpropanenitrile (1 g, 4.46 mmol) is dissolved in anhydrous THF (75 ml) the solution is cooled down to −100° C. with a diethyl ether-liquid nitrogen bath, n-butyl lithium 2M in c-hexane (4.0 ml, 8.0 mmol) is added and this reaction mixture stirred for 10 min., then N-methoxy-N-methyl acetamide (1.6 g, 15.6 mmol) is added and the reaction is then left to slowly warm-up to room temperature. After work-up (washing with acidic brine) and concentration the crude mixture is purified on silica gel using a 0 to 50% ethyl acetate in hexane gradient, to give the desired compound (660 mg, 78%) as a clear oil.

WORKUP

后处理

  1. waitthe reaction is then left
  2. temperatureto slowly warm-up to room temperature
  3. washAfter work-up (washing with acidic brine) and concentration the crude mixture
  4. customis purified on silica gel using a 0 to 50% ethyl acetate in hexane gradient