HRID9672

反应详情

EQUATION

反应方程式

HRID 9672 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of (3-methylthien-2-yl)methanol (3.20 g) in tetrahydrofuran (10 ml) was added to a mixture of sodium hydride (60% dispersion in mineral oil, 1.05 g) in tetrahydrofuran (40 ml). After the evolution of hydrogen had subsided triisopropylsilyl chloride (5.2 ml) was added. The reaction mixture was stirred for 2 hours then diluted with ethyl acetate. The mixture was extracted with water, 2M aqueous sodium hydroxide, water and dried with brine and over sodium sulfate. The crude product was purified by Biotage chromatography® using 100:1 petroleum ether:ethyl acetate as eluent to give the title compound as a colorless oil.

WORKUP

后处理

  1. additionwas added
  2. extractionThe mixture was extracted with water, 2M aqueous sodium hydroxide, water
  3. dry with materialdried with brine and over sodium sulfate
  4. customThe crude product was purified by Biotage chromatography®