HRID456264

反应详情

EQUATION

反应方程式

HRID 456264 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of tert-butyl (3R*,4S*)-3-(3-azidopropyl)-4-{(3-methylbutyl)[(4-nitrophenyl)sulfonyl]amino}pyrrolidine-1-carboxylate (0.55 g, 1.05 mmol) in toluene (50 mL), PPh3 (0.28 g, 1.05 mmol) was added and the mixture was heated at reflux for 1.5 hours. The mixture was diluted with 10 mL THF, H2O was added (28 mg, 1.57 mmol) and the reaction was heated at reflux for additional 1.5 hours. The solvents were evaporated and the residue was purified by column chromatography on silica gel eluting with 5→10% MeOH in CH2Cl2 giving the title compound.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 1.5 hours
  3. additionwas added (28 mg, 1.57 mmol)
  4. temperaturethe reaction was heated
  5. temperatureat reflux for additional 1.5 hours
  6. customThe solvents were evaporated
  7. customthe residue was purified by column chromatography on silica gel eluting with 5→10% MeOH in CH2Cl2 giving the title compound