HRID411253

反应详情

EQUATION

反应方程式

HRID 411253 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 0° C. solution of (S)—(+)-1,3-butanediol (2.1 g, 23.3 mmol), imidazole (1.74 g, 25.6 mmol), and N,N-dimethylformamide (1.0 mL) in dichloromethane (40 mL) was treated with tert-butyl-dimethylsilyl chloride (3.68 g, 23.3 mmol). The reaction mixture was warmed to room temperature, stirred overnight, quenched with saturated aqueous ammonium chloride and extracted with dichloromethane. The combined dichloromethane layers were dried (MgSO4), filtered and concentrated to afford of the desired product of sufficient purity for subsequent use without further purification in near quantitative yield.

WORKUP

后处理

  1. customquenched with saturated aqueous ammonium chloride
  2. extractionextracted with dichloromethane
  3. dry with materialThe combined dichloromethane layers were dried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated