HRID1696738

反应详情

EQUATION

反应方程式

HRID 1696738 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 7.3 g (3-methyl-thiophen-2-yl)-methanol in 65 ml tetrahydrofuran was added 2.73 g sodium hydride 55% in oil and the mixture was stirred at room temperature for 1 h. To ethe resulting mixture was added 4.3 ml iodomethane and the mixture was stirred at room temperature for 18 h. The reaction mixture was partitioned between aqueous potassium hydrogensulfate and ethyl acetate. The phases were separated and the organic phase was washed with water and brine dried over magnesium sulfate dehydrate and purified by distillation (13 mBar 160° C.) to yield 6.5 g of the title compound as light brown oil.

WORKUP

后处理

  1. stirringthe mixture was stirred at room temperature for 18 h
  2. customThe reaction mixture was partitioned between aqueous potassium hydrogensulfate and ethyl acetate
  3. customThe phases were separated
  4. washthe organic phase was washed with water and brine
  5. dry with materialdried over magnesium sulfate dehydrate
  6. distillationpurified by distillation (13 mBar 160° C.)