反应详情

A mixture of 5.3 parts of chloroacetonitrile, 14.4 parts of 3-(2-ethoxyethyl)-2-(1-piperazinylmethyl) -3H-imidazo[4,5-b]pyridine, 7.4 parts of sodium carbonate and 288 parts of N,N-dimethylformamide was stirred overnight at room temperature. The reaction mixture was stirred into water and the product was extracted with dichloromethane. The extract was dried, filtered and evaporated. The residue was purified by column chromatography over silica gel using a mixture of dichloromethane and methanol (95:5 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was stirred in 2,2'-oxybispropane. The product was filtered off and dried, yielding 13 parts (79.2%) of 4-[[3-(2-ethoxyethyl)-3H-imidazo[4,5-b]pyridin-2-yl]methyl]-1-piperazineacetonitrile; mp. 80.7° C. (compound 75).

1. extractionthe product was extracted with dichloromethane
2. customThe extract was dried
3. filtrationfiltered
4. customevaporated
5. customThe residue was purified by column chromatography over silica gel using
6. additiona mixture of dichloromethane and methanol (95:5 by volume) as eluent
7. customThe pure fractions were collected
8. customthe eluent was evaporated
9. stirringThe residue was stirred in 2,2'-oxybispropane
10. filtrationThe product was filtered off
11. customdried