HRID37219

反应详情

EQUATION

反应方程式

HRID 37219 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

1.6 g (0.053 mol) of sodium hydride (80%) are suspended under protective gas in 50 ml of DMF, 10 g (0.053 mol) of 2-butyl-5-formyl-4-chloroimidazole (preparation as described in EP 324,377) in 100 ml of DMF are added dropwise at 0° C., the mixture is subsequently stirred for 15 minutes at 0° C., and 18.9 g (0.053 mol) of tert-butyl 2-(4-bromomethylphenyl)-2-cyclopentyl-acetate in 100 ml of DMF are added dropwise. Stirring is continued for 2 hours at 0° C., the solvent is evaporated, the residue is taken up in diethyl ether, the mixture is filtered, and the product is concentrated and then chromatographed over silica gel 60 using dichloromethane. Yield: 16.2 g (66.7% of theory)

WORKUP

后处理

  1. stirringStirring
  2. waitis continued for 2 hours at 0° C.
  3. customthe solvent is evaporated
  4. filtrationthe mixture is filtered
  5. concentrationthe product is concentrated
  6. customchromatographed over silica gel 60 using dichloromethane