反应详情

A mixture of 1.7 parts of 2-chloropyrimidine, 5.5 parts of N-[1-(2 aminoethyl)-4-piperidinyl]-9-[(4-fluorophenyl)methyl]-9H-purin-8-amine, 1.5 parts of sodium hydrogen carbonate and 160 parts of ethanol was stirred and refluxed for 20 hours. The reaction mixture was evaporated. 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 acetonitrile, yielding 4.5 parts (67%) of 9-[(4-fluorophenyl)methyl]-N-[1-[2-(2-pyrimidinylamino)ethyl]-4-piperidinyl]-9H-purin-8-amine; mp. 164.1° C. (compound 164).

1. temperaturerefluxed for 20 hours
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 acetonitrile