HRID273178

反应详情

EQUATION

反应方程式

HRID 273178 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of (R)-1-[4-(3-fluoro-benzyloxy)-phenyl]-5-oxo-pyrrolidine-3-carboxylic acid amide (0.400 g, 0.001 mol) and thionyl chloride (2.3 ml, 0.032 mol) was refluxed under argon for 3 hours. The mixture was cooled to room temperature, diluted with 5 ml tetrahydrofuran, concentrated under vacuum and purified by column chromatography on silica gel using a 2:3-mixture of ethyl acetate and hexane as the eluent. The product fractions were concentrated to dryness to yield (0.106 g, 28% of theory) of a light brown oil. MS (m/e)=311.1 (M+H)+.

WORKUP

后处理

  1. temperaturewas refluxed under argon for 3 hours
  2. concentrationconcentrated under vacuum
  3. custompurified by column chromatography on silica gel using a 2
  4. concentrationThe product fractions were concentrated to dryness
  5. customto yield (0.106 g, 28% of theory) of a light brown oil