HRID2173829

反应详情

EQUATION

反应方程式

HRID 2173829 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A cooled solution (0° C. by internal thermometer) of (S,S)-2-methyl-N-(3-methyl-1-{4-[5-(trifluoromethyl)pyridin-2-yl]phenyl}butyl)propane-2-sulfinamide (74.0 g, 179 mmol) in methanol (0.90 L) was treated with 2.0M hydrochloric acid in diethylether (233 ml, 466 mmol) dropwise while maintaining the reaction temperature below 15° C. Following 1 hour, the solvent was removed in vacuo and the resulting oil was treated with diethylether to precipitate the product as a fine white solid. The solid was collected via filtration, and washed with diethylether (3×100 ml). The remaining solid was dried in vacuo. The crude material was used for further transformations.

WORKUP

后处理

  1. temperaturewhile maintaining the reaction temperature below 15° C
  2. customthe solvent was removed in vacuo
  3. additionthe resulting oil was treated with diethylether
  4. customto precipitate the product as a fine white solid
  5. filtrationThe solid was collected via filtration
  6. washwashed with diethylether (3×100 ml)
  7. customThe remaining solid was dried in vacuo