HRID238968

反应详情

EQUATION

反应方程式

HRID 238968 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

3-[3-(3-Trifluoromethoxy-benzenesulfonylamino)-phenyl]-pyrrolidine-1-carboxylic acid methyl ester (0.105 g; 0.24 mmol) were dissolved in 2.5 ml ethanol and 0.9 ml of concentrated HCl were added. The reaction mixture was heated in a microwave system (CEM) at 90-150° C. for several hours until consumption of starting material. The mixture was then concentrated in vacuo and the acidic aqueous phase extracted twice with diethylether. The aqueous phase was adjusted to pH 9 with 1 N aqueous NaOH, extracted three times with diethylether, and the combined organic layers dried over sodium sulfate, filtered and the solvent evaporated to dryness to yield 45 mg of the product.

WORKUP

后处理

  1. concentrationThe mixture was then concentrated in vacuo
  2. extractionthe acidic aqueous phase extracted twice with diethylether
  3. extractionextracted three times with diethylether
  4. dry with materialthe combined organic layers dried over sodium sulfate
  5. filtrationfiltered
  6. customthe solvent evaporated to dryness