HRID2209840

反应详情

EQUATION

反应方程式

HRID 2209840 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 13.2 g (113 mmol) of (5S)-dihydro-5-(hydroxymethyl)furan-2(3H)-one in 200 ml of dimethyiformamide was treated sequentially with 9.28 g (136 mmol) of imidazole and 18.84 g (125 mmol) of chloro-t-butyldimethylsilane, the latter in several portions. The resulting solution was stirred at ambient temperature for 6 h, poured into 10% aqueous citric acid, and extracted with ethyl acetate. The organic layer was washed sequentially with two portions of water, one portion of aqueous NaHCO3 and one portion of saturated brine. The organic layer was dried over MgSO4, and concentrated in vacuo to provide 22.04 g (90%) of the desired compound.

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed sequentially with two portions of water, one portion of aqueous NaHCO3 and one portion of saturated brine
  3. dry with materialThe organic layer was dried over MgSO4
  4. concentrationconcentrated in vacuo