HRID1195377

反应详情

EQUATION

反应方程式

HRID 1195377 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3,3-bis(2-fluoro-4-methylphenyl)-2-(1-methyl-1H-tetrazol-5-yl)-2-propenal (1.35 g, 3.8 mmoles) and triphenylphosphoranylidene acetaldehyde (1.16 g, 3.8 mmoles) in benzene was heated at reflux for 3 hours. The solvent was removed and the residue purified by column chromatography on silica gel eluting with 1% (v/v) methanol in methylene chloride. The fractions containing material having Rf =0.9 [methanol-methylene chloride; 1:20 (v/v)] were combined and concentrated to give 1.3 g of the title compound; m.p.=88°-108° C.

WORKUP

后处理

  1. temperatureat reflux for 3 hours
  2. customThe solvent was removed
  3. customthe residue purified by column chromatography on silica gel eluting with 1% (v/v) methanol in methylene chloride
  4. additionThe fractions containing material
  5. concentrationconcentrated