HRID2372437

反应详情

EQUATION

反应方程式

HRID 2372437 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The Gringnard reagent, diphenylethanyl magnesium chloride, is prepared by the usual way from diphenylethanylchloride (0.01 mol) and magnesium turnings (0.01 mol) in dry diethylether (30 ml). 1-benzyl-5-imidazole aldehyde (0.005 mol) is dissolved in dry diethylether and the Grignard reagent is added dropwise to the solution. The reaction mixture is refluxed for 3 hours. The reaction is then poured into 2N hydrochloric acid and extracted with diethylether. The water phase is made basic with sodium hydroxide and then extracted with ethyl acetate. The ethyl acetate phase is dried and evaporated. The residue is purified by flash-chromatography eluating with methylene chloride-methanol mixture (9.5:0.5). M.p. of the product as base is 188°-190° C.

WORKUP

后处理

  1. temperatureThe reaction mixture is refluxed for 3 hours
  2. extractionextracted with diethylether
  3. extractionextracted with ethyl acetate
  4. dry with materialThe ethyl acetate phase is dried
  5. customevaporated
  6. customThe residue is purified by flash-chromatography
  7. customis 188°-190° C.