HRID1955736

反应详情

EQUATION

反应方程式

HRID 1955736 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% strength) are suspended in 50 ml of DMF under protective gas, 10 g (0.053 mol) of 2-butyl-5-formyl-4-chloroimidazole (preparation according to EP 324,377) in 100 ml of DMF are added dropwise at 0° C., the mixture is then stirred at 0° C. for 15 min and 18.9 g (0.053 mol) of tert-butyl 2-(4-bromomethylphenyl-2-cyclopentylacetate in 100 ml of DMF are added dropwise. The mixture is stirred at 0° C. for 2 h, the solvent is evaporated, the residue is taken up in diethyl ether and filtered and, after concentration, chromatographed on silica gel 60 using dichloromethane.

WORKUP

后处理

  1. additionare added dropwise at 0° C.
  2. stirringThe mixture is stirred at 0° C. for 2 h
  3. customthe solvent is evaporated
  4. filtrationfiltered
  5. concentrationafter concentration
  6. customchromatographed on silica gel 60 using dichloromethane