HRID1249678

反应详情

EQUATION

反应方程式

HRID 1249678 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A solution of ethyl (4′-biphenyl)acetate (7.1 g) in 60 ml of diethylcarbonate, kept under nitrogen atmosphere, is added portionwise with sodium (0.734 g), then it is heated at 120° C. for 3 hours. The solvent is evaporated off and the residue is dissolved in 65 ml of cold water and acidified with acetic acid until pH=5-6 is reached. The aqueous phase is then extracted three times with diethyl ether and the pooled organic extracts are dried over sodium sulfate and concentrated to dryness. The residue is purified by silica gel chromatography (eluent: petroleum ether/diethyl ether 9.4:0.6) to give 7.05 g of the product. m.p. 51-53° C.

WORKUP

后处理

  1. customThe solvent is evaporated off
  2. dissolutionthe residue is dissolved in 65 ml of cold water
  3. extractionThe aqueous phase is then extracted three times with diethyl ether
  4. dry with materialthe pooled organic extracts are dried over sodium sulfate
  5. concentrationconcentrated to dryness
  6. customThe residue is purified by silica gel chromatography (eluent: petroleum ether/diethyl ether 9.4:0.6)