HRID22262

反应详情

EQUATION

反应方程式

HRID 22262 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. filtrationThe mixture was filtered
  2. washthe solid washed with a mixture of 1:1 ethanol/isopropanol, solvent
  3. customevaporated from the filtrate
  4. customthe residue flash-chromatographed on silica gel
  5. washeluting with 2% methanol in dichloromethane