HRID2240238

反应详情

EQUATION

反应方程式

HRID 2240238 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 100 mg (0.25 mmol) of N-(2-fluoro-4-nitrophenyl)-1-{[2-(trimethyl-silyl)ethoxy]methyl}-1H-pyrrolo[2,3-b]pyridine-4-amine in 0.75 ml of DMA is added dropwise to a suspension of 30 mg (0.75 mmol) of sodium hydride in 0.75 ml of DMA, and the mixture is stirred at RT for 30 min. 77 μl (1.24 mmol) of methyl iodide are then slowly added dropwise, and the mixture is stirred for a further 30 min. Water is then added, and the mixture is extracted twice with dichloromethane. The combined organic phases are dried over magnesium sulfate, the solvent is removed under reduced pressure and the residue is purified by preparative HPLC.

WORKUP

后处理

  1. stirringthe mixture is stirred for a further 30 min
  2. extractionthe mixture is extracted twice with dichloromethane
  3. dry with materialThe combined organic phases are dried over magnesium sulfate
  4. customthe solvent is removed under reduced pressure
  5. customthe residue is purified by preparative HPLC