HRID1906980

反应详情

EQUATION

反应方程式

HRID 1906980 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

(trans)-3-(6-Phenyl-1,3,5-hexatriynyl)oxiranecarboxaldehyde (80 mg, 0.36 mmole; see example 4) and formylmethylenetriphenylphosphorane (122 mg, 0.40 mmole) were dissolved in 10 ml of dry benzene and the mixture was heated at 70° C. for 10 minutes. The mixture was then cooled to room temperature and the solvent was removed in vacuo. The residue was taken up in ether and filtered through a plug of silica gel. Removal of solvent afforded a brown oil which was purified by chromatography (silica gel, ether-hexane 1:1) to afford 46 mg of the title compound, melting point 91°-92.5° C.

WORKUP

后处理

  1. temperatureThe mixture was then cooled to room temperature
  2. customthe solvent was removed in vacuo
  3. filtrationfiltered through a plug of silica gel
  4. customRemoval of solvent
  5. customafforded a brown oil which
  6. customwas purified by chromatography (silica gel, ether-hexane 1:1)