反应详情

A mixture of 1.65 parts of 2-(phenoxymethyl)oxirane, 8.9 parts of 3-(2-ethoxyethyl)-2-(1-piperazinylmethyl)-3H-imidazo[4,5-b]pyridine and 40 parts of 2-propanol was stirred for 20 hours at reflux temperature. The reaction mixture was evaporated and the residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol (95:5 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was crystallized from 2,2'-oxybispropane. The product was filtered off and dried, yielding 1.36 parts (31.0%) of 4-[[3-(2-ethoxyethyl)3H-imidazo[4,5-b]pyridin-2-yl]methyl]-α-(phenoxymethyl)-1-piperazineethanol; mp. 102.5° C. (compound 118).

1. temperatureat reflux temperature
2. customThe reaction mixture was evaporated
3. customthe residue was purified by column chromatography over silica gel using
4. additiona mixture of trichloromethane and methanol (95:5 by volume) as eluent
5. customThe pure fractions were collected
6. customthe eluent was evaporated
7. customThe residue was crystallized from 2,2'-oxybispropane
8. filtrationThe product was filtered off
9. customdried