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 (N-{4-[4-(3-Trifluoromethyl-phenyl)-1H-imidazol-2-yl]-cyclohexylmethyl}-acetamide (207 mg, 0.57 mmol, from Example 2A) in THF, 3 equivalents of borane dimethylsulfide (2M in THF) was added, and the solution stirred overnight at room temperature. One volume of MeOH was added to the reaction mixture, and the mixture was concentrated under reduced pressure. 50 mL of 3N HCl was added, and the mixture was warmed for 5 minutes. After washing the solution with ether, the solution was made basic with NaOH and extracted with ethyl acetate. The solution was dried (Na2SO4), concentrated under reduced pressure, and purified using preparative plate chromatography to give Ethyl-{4-[4-(3-trifluoromethyl-phenyl)-1H-imidazole-2-yl]cyclohexylmethyl}-amine.
WORKUP
后处理
- concentrationthe mixture was concentrated under reduced pressure
- addition50 mL of 3N HCl was added
- temperaturethe mixture was warmed for 5 minutes
- washAfter washing the solution with ether
- extractionextracted with ethyl acetate
- dry with materialThe solution was dried (Na2SO4)
- concentrationconcentrated under reduced pressure
- custompurified