HRID2262610

反应详情

EQUATION

反应方程式

HRID 2262610 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-[3-(4-Trifluoromethoxy-benzenesulfonylamino)-phenyl]-pyrrolidine-1-carboxylic acid methyl ester (500 mg, 1.13 mmol) and HCl (8M, 137.82 mmol) in EtOH (10 ml) were heated under reflux for 48 h. The mixture was extracted twice with ethyl acetate and then NaOH (2M) was added. The aqueous phase was extracted twice with ethyl acetate. The combined organic layers were washed with water and saturated sodium chloride solution, dried over MgSO4 and evaporated under reduced pressure to give the product as a brown oil (200 mg, 46%).

WORKUP

后处理

  1. temperatureunder reflux for 48 h
  2. extractionThe mixture was extracted twice with ethyl acetate
  3. additionNaOH (2M) was added
  4. extractionThe aqueous phase was extracted twice with ethyl acetate
  5. washThe combined organic layers were washed with water and saturated sodium chloride solution
  6. dry with materialdried over MgSO4
  7. customevaporated under reduced pressure