反应详情

Grams 10.9 of 2,3-diaminopyridine and 17,9 g N-methylnipecotic acid hydrochloride are heated at 190° C. for 6 hours. The reaction mixture is cooled and diluted with a small amount of water, then is made alkaline to pH 10 by addition of NaOH and extraction is repeated several times with methylene chloride. The organic extracts, collected together, are evaporated to dryness. The obtained residue, is extracted several times with diethyl ether and the ethereal extracts are evaporated to dryness. The obtained residue, crystallized from acetonitrile, provides 5 g (23% of the theoretical value) 2-(1-methylpiperidin-3-yl)-3H-imidazo-[4,5-b] pyridine melting at 141°-144° C.

1. temperatureThe reaction mixture is cooled
2. customThe organic extracts, collected together
3. customare evaporated to dryness
4. extractionThe obtained residue, is extracted several times with diethyl ether
5. customthe ethereal extracts are evaporated to dryness
6. customThe obtained residue, crystallized from acetonitrile