HRID1789028

反应详情

EQUATION

反应方程式

HRID 1789028 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ethyl 4-fluoro-3-oxobutanoate (1.45 g, 10 mmoles), ethyl 2-(3-nitrophenylmethylene)-3-oxobutanoate (2.63 g, 10 mmoles) and aqueous ammonia (1.1 ml, d 0.88) were heated at reflux in ethanol (15 ml) for 6 hours. The solvent was removed in vacuo and the residue purified by chromatography on silica eluting with petroleum ether (60°-80° )/ether mixtures. Recrystallisation from ether/petroleum ether (60°-80° ) gave the title compound (1.1 g) as yellow crystals mp 139°-41°.

WORKUP

后处理

  1. customThe solvent was removed in vacuo
  2. customthe residue purified by chromatography on silica eluting with petroleum ether (60°-80° )/ether mixtures
  3. customRecrystallisation from ether/petroleum ether (60°-80° )