反应详情

温度

102.5 °C

Sulfone 11.1 (0.400 g, 1.18 mmol) was combined with trans-4-aminocyclohexanol (0.272 g, 2.36 mmol) and 2-methoxyethyl ether (0.4 mL). The mixture was heated to 100-105° C. for 1 hour at which time it was cooled to room temperature and concentrated in vacuo. The residue was purified by column chromatography on silica gel using 9:1 dichloromethane/methanol. The column fractions containing product were combined and concentrated in vacuo to an oil which was re-dissolved in ethyl acetate and methanol. Addition of hydrochloric acid (1.0M/Et2O, 1.0 equivalent) gave the salt which dissolved in the solvents. The solution was concentrated in vacuo to a solid which was triturated in ether, filtered and dried to give 0.220 g of 3-(2-chlorophenyl)-7-(trans-4-hydroxycyclohexylamino)-3,4-dihydropyrimido[4,5-d]pyrimidin-2(1H)-one.

1. temperaturewas cooled to room temperature
2. concentrationconcentrated in vacuo
3. customThe residue was purified by column chromatography on silica gel using 9:1 dichloromethane/methanol
4. additionThe column fractions containing product
5. concentrationconcentrated in vacuo to an oil which
6. dissolutionwas re-dissolved in ethyl acetate
7. customgave the salt which
8. dissolutiondissolved in the solvents
9. concentrationThe solution was concentrated in vacuo to a solid which
10. customwas triturated in ether
11. filtrationfiltered
12. customdried