反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- concentrationThe reaction medium is concentrated under reduced pressure
- customThe residue obtained
- filtrationfiltered through Celite
- concentrationThe filtrate is concentrated under reduced pressure
- customthe residue obtained
- customis purified by flash-pack chromatography (SiO2, dichloromethane/methanol 95/05 by volume as eluents)