HRID1911523

反应详情

EQUATION

反应方程式

HRID 1911523 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of crude (R)-2,2-dimethyl-4-(1-methyl-1-phenoxythiocarbonyloxy-2-phenyl-ethyl)-oxazolidine-3-carboxylic acid tert-butyl ester (700 mg) in toluene (5 ml) was treated under an argon atmosphere with 2,2′ azobis(2-methylproponitrile) (122 mg) and tri-N-butyltin hydride (0.79 ml). The reaction mixture was refluxed for 30 min, then cooled to r.t. and then directly purified by column chromatography (silica gel, gradient: cyclohexane ->cyclohexane/EtOAc 10:1) to give (S)-2,2-dimethyl-4-(1-methyl-2-phenyl-vinyl)-oxazo-lidine-3-carboxylic acid tert-butyl ester (279 mg, 59%) as light yellow waxy solid. MS (ISP): 318.3 ([M+H]+))

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed for 30 min
  2. customdirectly purified by column chromatography (silica gel, gradient: cyclohexane ->cyclohexane/EtOAc 10:1)