HRID1635938
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 2.0 g(13.5 mmol) of 4-methyl-5-imidazolemethanol hydrochloride and 1.95 g(14.17 mmol) of potassium carbonate in 20 ml of dimethylformamide was added 3.88 g(14.17 mmol) of t-butyldiphenylsilylchloride was added dropwise thereto, and the resulting mixture was stirred for 3 hours. The solvent was removed under reduced pressure and the residue was dissolved in 20 ml of ethylacetate. The organic layer was washed with 20 ml of saturated aqueous sodium bicarbonate solution, dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to column chromatography(eluent: dichloromethane/methanol=95/5, v/v) to give 1.22 g(3.44 mmol, Yield 26%) of the title compound.
WORKUP
后处理
- additionwas added dropwise
- customThe solvent was removed under reduced pressure
- dissolutionthe residue was dissolved in 20 ml of ethylacetate
- washThe organic layer was washed with 20 ml of saturated aqueous sodium bicarbonate solution
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated