反应详情

温度

70 °C

A mixture of 3.2 parts of 2,3-dihydro-1,4-benzodioxin-2-methanol 4-methylbenzenesulfonate (ester), 4.5 parts of 7-[(4-fluorophenyl)methyl]-8-(4-piperidinylmethyl)-7H-purin-6-ol dihydrobromide, 4 parts of sodium carbonate and 45 parts of N,N-dimethylformamide was stirred overnight at 70° C. After cooling, the reaction mixture was filtered over diatomaceous earth and the filtrate was 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 1.5 parts (34%) of 8-[[1-[(2,3-dihydro-1,4-benzodioxin-2-yl)methyl]-4-piperidinyl]methyl]-7-[(4-fluorophenyl)methyl]-7H-purin-6-ol; mp. 175.2° C. (compound 59).

1. temperatureAfter cooling
2. filtrationthe reaction mixture was filtered over diatomaceous earth
3. customthe filtrate was evaporated
4. customThe residue was purified by column chromatography over silica gel using
5. additiona mixture of trichloromethane and methanol
6. customThe pure fractions were collected
7. customthe eluent was evaporated
8. customThe residue was crystallized from acetonitrile
9. filtrationThe product was filtered off
10. customdried