HRID727539

反应详情

EQUATION

反应方程式

HRID 727539 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

A solution of 3-(2-methylpropyl)-1-trimethylsilyl-2-pyrrolidinone (10.2 g, 47.8 mmol) and THF (153 mL) is cooled to -78° C., and LDA (2.0 M, 26.3 mL, 52.6 mmol) is added. The solution is stirred at -78° C. for 30 minutes and then allyl bromide (5.0 mL, 57 mmol) is added. The solution is allowed to warm to 5° C. over 2.5 hours, and is then stirred at 5° C. for 1 hour. After quenching with saturated aqueous ammonium chloride (25 mL), aqueous workup (EtOAc, MgSO4) and purification by column chromatography (1:9:10 v/v CH2Cl2 :EtOAc:hexane) provides 7.76 g (90%) of the title compound as an oil.

WORKUP

后处理

  1. temperatureto warm to 5° C. over 2.5 hours
  2. stirringis then stirred at 5° C. for 1 hour
  3. customAfter quenching with saturated aqueous ammonium chloride (25 mL), aqueous workup (EtOAc, MgSO4) and purification by column chromatography (1:9:10 v/v CH2Cl2 :EtOAc:hexane)