HRID506836

反应详情

EQUATION

反应方程式

HRID 506836 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

To a solution of 0.5 g of [2-(5,6-dimethoxy-1-methyl-1H-pyrrolo[3,2-b]pyridin-3-yl)-1-(toluene-4-sulfonyl)-1H-pyrrolo[2,3-b]pyridin-4-carbaldehyde oxime in 30 cm3 of ethanol and 25 cm3 of water, at a temperature in the region of 20° C., are added 0.65 g of zinc and 17.5 cm3 of concentrated formic acid. The reaction medium is stirred at room temperature for 8 days. The reaction medium is concentrated under reduced pressure. The residue obtained is taken up in methanol, basified with sodium hydroxide (30%) to pH=9-10 and then filtered through Celite. The filtrate is concentrated under reduced pressure and the residue obtained is purified by flash-pack chromatography (SiO2, dichloromethane/methanol 95/05 by volume as eluents). 0.1 g of [2-(5,6-dimethoxy-1-methyl-1H-pyrrolo[3,2-b]pyridin-3-yl)-1-(toluene-4-sulfonyl)-1H-pyrrolo[2,3-b]pyridin-4-yl]methylamine is obtained with the following characteristics:

WORKUP

后处理

  1. concentrationThe reaction medium is concentrated under reduced pressure
  2. customThe residue obtained
  3. filtrationfiltered through Celite
  4. concentrationThe filtrate is concentrated under reduced pressure
  5. customthe residue obtained
  6. customis purified by flash-pack chromatography (SiO2, dichloromethane/methanol 95/05 by volume as eluents)