反应详情

1.20 g (4.35 mmol) 2-(2-Chloro-pyridin-4-yl)-6-nitro-3H-imidazo[4,5-b]pyridine in 12 ml dry NMP and 1.18 g (13 mmol) 3-methoxypropylamine were heated to 200° C. in a closed vessel in a microwave reactor for 30 min. The solvent was removed under vacuum and the residue dissolved in a mixture of 20 ml ethyl acetate and 30 ml 5% aqueous HCl. The HCl phase was separated and brought to alkaline pH by addition of conc. ammonia. The alkaline aqueous phase was extracted with dichloromethane, and the organic phases were combined and dried. Evaporation and chromatography of the residue on silica in ethyl acetate/methanol mixtures gave 480 mg of the title product.

1. customThe solvent was removed under vacuum
2. dissolutionthe residue dissolved in a mixture of 20 ml ethyl acetate and 30 ml 5% aqueous HCl
3. customThe HCl phase was separated
4. additionbrought to alkaline pH by addition of conc. ammonia
5. extractionThe alkaline aqueous phase was extracted with dichloromethane
6. customdried
7. customEvaporation and chromatography of the residue on silica in ethyl acetate/methanol