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
- 0 °C
PROCEDURE
实验过程
Benzyl 3-chloroformylpropionate was prepared from benzyl hydrogen succinate (1.96 g) and oxalyl chloride (0.9 ml) in an usual manner. A solution of sodium phenolate, which was prepared from phenol (1.77 g) and sodium hydride (60% dispersion in mineral oil, 1.13 g) in tetrahydrofuran (20 ml), was added to a solution of the acid chloride in tetrahydrofuran (20 ml) at 0° C. After stirred at 0° C. for 30 minutes, the mixture was poured into a mixture of ethyl acetate and 1N hydrochloric acid. The organic layer was separated, washed with water, and dried over magnesium sulfate After evaporation of the solvent, the residue was chromatographed on silica gel (50 g) eluting with a mixture of ethyl acetate and hexane (1:10→1:5) to give benzyl phenyl succinate (2.15 g) as colorless crystals.
WORKUP
后处理
- customThe organic layer was separated
- washwashed with water
- dry with materialdried over magnesium sulfate
- customAfter evaporation of the solvent
- customthe residue was chromatographed on silica gel (50 g)
- washeluting with a mixture of ethyl acetate and hexane (1:10→1:5)