HRID23574

反应详情

EQUATION

反应方程式

HRID 23574 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 2-nitro-N-(2-oxo-1-(S)-phenyl-2-pyrrolidin-1-yl-ethyl)-benzenesulfonamide (62.4 g, 160 mmol) in anhydrous dimethylformamide (300 cm3) was added potassium carbonate (44.3 g, 320 mmol). The mixture was stirred at ambient temperature for 10 minutes and allyl bromide (18.0 cm3, 208 mmol) was added dropwise over 10 minutes. The mixture was stirred for 16 hours at ambient temperature and poured into water (2000 cm3) to afford a white precipitate. The mixture was vacuum filtered, washed with water (3×200 cm3) and vacuum dried at 50° C. to constant weight to afford the title compound as a white solid (66.2 g, 96.2%) with a positive ion ESI (M−H)+430.2.

WORKUP

后处理

  1. stirringThe mixture was stirred for 16 hours at ambient temperature
  2. customto afford a white precipitate
  3. filtrationfiltered
  4. washwashed with water (3×200 cm3) and vacuum
  5. customdried at 50° C. to constant weight