HRID1249678
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe solvent is evaporated off
- dissolutionthe residue is dissolved in 65 ml of cold water
- extractionThe aqueous phase is then extracted three times with diethyl ether
- dry with materialthe pooled organic extracts are dried over sodium sulfate
- concentrationconcentrated to dryness
- customThe residue is purified by silica gel chromatography (eluent: petroleum ether/diethyl ether 9.4:0.6)