HRID421293

反应详情

EQUATION

反应方程式

HRID 421293 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

400 mg of sodium hydride (60% in oil, 10 mmol) were added to a stirred solution of 4.4 g of ethoxycarbonylmethyltriphenylphosphonium bromide (10 mmol) in 20 ml of DMF and the mixture was stirred further at RT for 10 min. 1.24 g of 2-fluoro-benzaldehyde (10 mmol) were added and the mixture was stirred for 5 h at RT. The reaction mixture was taken up in 100 ml of ethyl acetate and washed with a common salt solution, dried over sodium sulfate, filtered and concentrated under reduced pressure. Purification took place using a silica gel chromatography (ethyl acetate/heptane 1:1). 1.25 g of the title compound were obtained. Yield: 60%.

WORKUP

后处理

  1. stirringthe mixture was stirred for 5 h at RT
  2. washwashed with a common salt solution
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customPurification