HRID2192172

反应详情

EQUATION

反应方程式

HRID 2192172 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

50 mg (0.10 mmol) of N-[3-fluoro-4-({3-(2-hydroxyethyl)-1-[(4-methylphenyl)sulfonyl]-1H-pyrrolo-[2,3-b]pyridin-4-yl}oxy)phenyl]acetamide are initially charged in 2.0 ml of dichloromethane. 25 μl (0.31 mmol) of pyridine and 19.7 mg (0.10 mmol) of p-toluenesulfonyl chloride are added, and the mixture is stirred at RT overnight. Two more times, the same amounts of pyridine and p-toluenesulfonyl chloride are added, at intervals of 2 hours. After the reaction has come to completion, the reaction solution is diluted with ethyl acetate and extracted twice with saturated ammonium chloride solution. The organic phase is dried over magnesium sulfate and the solvent is removed under reduced pressure. The crude product is purified by preparative HPLC.

WORKUP

后处理

  1. extractionextracted twice with saturated ammonium chloride solution
  2. dry with materialThe organic phase is dried over magnesium sulfate
  3. customthe solvent is removed under reduced pressure
  4. customThe crude product is purified by preparative HPLC