反应详情

A mixture of 1.2 parts of bromo-1-propene, 3.26 parts of 9-[(4-fluorophenyl)methyl]-N-(4-piperidinyl)-9H-purin-8-amine, 1.5 parts of sodium hydrogen carbonate and 40 parts of ethanol was stirred for 1 hour at reflux temperature. The reaction mixture was filtered over diatomaceous earth while hot and the filtrate was evaporated. The residue was taken up in water and the product was extracted with 4-methyl-2-pentanone. The extract was dried, filtered and evaporated. The residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol, saturated with ammonia, (95:5 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was crystallized from acetonitrile. The product was filtered off and dried, yielding 0.8 parts (22%) of 9-[(4-fluorophenyl)methyl]-N-[1-(2-propenyl)-4-piperidinyl)-9H-purin-8-amine; mp. 144.8° C. (compound 120).

1. temperatureat reflux temperature
2. filtrationThe reaction mixture was filtered over diatomaceous earth while hot and the filtrate
3. customwas evaporated
4. extractionthe product was extracted with 4-methyl-2-pentanone
5. customThe extract was dried
6. filtrationfiltered
7. customevaporated
8. customThe residue was purified by column chromatography over silica gel using
9. additiona mixture of trichloromethane and methanol
10. customThe pure fractions were collected
11. customthe eluent was evaporated
12. customThe residue was crystallized from acetonitrile
13. filtrationThe product was filtered off
14. customdried