HRID2423176

反应详情

EQUATION

反应方程式

HRID 2423176 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To N-(2-{[1-(phenylsulfonyl)-1H-indol-5-yl]oxy}ethyl)acetamide (Intermediate 25, 5.0 g, 14 mmol) in acetonitrile (7.5 L) was phosphoryl chloride (100 mL) added and the reaction mixture was heated at reflux overnight. The reaction mixture was allowed to cool to room temperature and the solvent was removed under reduced pressure to give the crude material of the title compound (5.0 g). A small amount of the crude material was purified by preparative HPLC (XTerra C18, 50 mM NH4HCO3 pH 10-CH3CN) to give the title compound (12 mg). MS m/z 341 [M+H]+.

WORKUP

后处理

  1. additionadded
  2. temperaturethe reaction mixture was heated
  3. temperatureat reflux overnight
  4. customthe solvent was removed under reduced pressure