反应 #1797558

反应方程式

compound B5

N,N-dimethyl-4-{2-[2-(7-oxo-azepan-2-yl)-ethyl]-3H-imidazo[4,5-b]pyridin-6-yl}-benzenesulfonamide

Lawesson's reagent

N,N-dimethyl-4-{2-[2-(7-oxo-azepan-2-yl)-ethyl]-3H-imidazo[4,5-b]pyridin-6-yl}-benzenesulfonamide

→

title compound

收率 63.6%

N,N-Dimethyl-4-{2-[2-(7-thioxo-azepan-2-yl)-ethyl]-3H-imidazo[4,5-b]pyridin-6-yl}-benzenesulfonamide

收率 63.6%

反应条件

后处理

1. 1
   其他The title compound is synthesized
2. 2
   其他Purification by chromatography on flash silica gel (eluent gradient: dichloromethane/0-5 vol. % ethanol)

实验过程

The title compound is synthesized as described for 7-[2-(6-{4-cyano-phen-1-yl}-3H-imidazo[4,5-b]pyridin-2-yl)-ethyl]-azepan-2-thione (compound A2) from 85 mg of N,N-dimethyl-4-{2-[2-(7-oxo-azepan-2-yl)-ethyl]-3H-imidazo[4,5-b]pyridin-6-yl}-benzenesulfonamide (compound B5) and 82 mg of Lawesson's reagent. Purification by chromatography on flash silica gel (eluent gradient: dichloromethane/0-5 vol. % ethanol) affords 56 mg of the title compound as a light yellow, waxy solid. ESI-MS: 458.3 (MH+). TLC: Rf=0.46 (dichloromethane/ethanol 10:1 parts by volume).

来源