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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
A solution of lithium aluminum hydride (0.6 g) and 1-(2,3,4-trimethoxyphenyl)methyl-4-[(2-(4-trifluoromethylphenyl)-1,5-dimethylimidazol-4-yl)-3-oxoprop-1-yl]piperazine (2 g) in 50 ml of tetrahydrofuran was refluxed for 48 hours Excess reagent was hydrolysed by cooling the mixture to 0° C. and adding wet tetrahydrofuran dropwise. The mixture was filtered, the solid washed with a mixture of 1:1 ethanol/isopropanol, solvent evaporated from the filtrate, and the residue flash-chromatographed on silica gel, eluting with 2% methanol in dichloromethane, to yield 400 mg of 1-(2,3,4-trimethoxyphenyl)methyl-4-[(2-(4-trifluoromethylphenyl)-1,5-dimethylimidazol-4-yl)prop-1-yl]piperazine, which was converted to its hydrochloride salt, m.p. 212° C.
WORKUP
后处理
- filtrationThe mixture was filtered
- washthe solid washed with a mixture of 1:1 ethanol/isopropanol, solvent
- customevaporated from the filtrate
- customthe residue flash-chromatographed on silica gel
- washeluting with 2% methanol in dichloromethane