HRID417421

反应详情

EQUATION

反应方程式

HRID 417421 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

The mixture of 2-[2-(4-Bromo-phenyl)-2-oxo-ethylcarbamoyl]-pyrrolidine-1-carboxylic acid tert-butyl ester (1.0 g, 2.44 mmol) and Lawesson's reagent (1.23 g, 3.0 mmol) in THF (16 ml) was heated at 80° C. for 4 hours. The solvent was removed under reduced pressure and the mixture was diluted with EtOAc. The organic phase was washed with saturated sodium bicarbonate, water, and brine, and was dried with sodium sulfate. Concentration and purification by flash column chromatography (hexanes/EtOAc) gave 2-[5-(4-Bromo-phenyl)-thiazol-2-yl]-pyrrolidine-1-carboxylic acid tert-butyl ester (655 mg). m/z: 410.7 (M+H)+.

WORKUP

后处理

  1. customThe solvent was removed under reduced pressure
  2. additionthe mixture was diluted with EtOAc
  3. washThe organic phase was washed with saturated sodium bicarbonate, water, and brine
  4. dry with materialwas dried with sodium sulfate
  5. concentrationConcentration and purification by flash column chromatography (hexanes/EtOAc)