HRID1353040

反应详情

EQUATION

反应方程式

HRID 1353040 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Tin(II) chloride (4.77 g) was added to a solution of ethyl 3-benzenesulphonylamino3-(3-nitrophenyl)-propionate from II.4a (2.0 g) in 60 ml of ethanol and the reaction mixture was heated under reflux for 2 h. After cooling, the solution was hydrolysed on ice and an NaHCO3 solution (5%) was added to pH=8. The mixture was then extracted with dichloromethane, and the org. phase was washed with NaCl, dried (MgSO4) and concentrated. A yellow oil was obtained (yield: 1.79 g).

WORKUP

后处理

  1. temperaturethe reaction mixture was heated
  2. temperatureunder reflux for 2 h
  3. temperatureAfter cooling
  4. extractionThe mixture was then extracted with dichloromethane
  5. washphase was washed with NaCl
  6. dry with materialdried (MgSO4)
  7. concentrationconcentrated
  8. customA yellow oil was obtained (yield: 1.79 g)