HRID1696738
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- stirringthe mixture was stirred at room temperature for 18 h
- customThe reaction mixture was partitioned between aqueous potassium hydrogensulfate and ethyl acetate
- customThe phases were separated
- washthe organic phase was washed with water and brine
- dry with materialdried over magnesium sulfate dehydrate
- distillationpurified by distillation (13 mBar 160° C.)