反应详情

温度

122.5 °C

A mixture of 1-Propyl-8-[1-(3-trifluoromethyl-benzyl)-1H-pyrazol-4-yl]-3,7-dihydro-purine-2,6-dione (7.2 g, 0.017 mol), NH4Cl (4.54 g, 0.085 mol) and POCl3 (220 ml) were heated at 120-125° C. for 72 h. Reaction mixture was cooled to 20-25° C. It was then concentrated under vacuum and quenched with cold water slowly and solid material was separated. It was filtered off and washed with water. The solid material was dried under vacuum. The crude product was purified by column chromatography using silica gel (230-400 mesh) and 0.5 to 4% methanol in chloroform as an eluent to obtain 2-Chloro-1-propyl-8-[1-(3-trifluoromethyl-benzyl)-1H-pyrazol-4-yl]-1,7-dihydro-purin-6-one (4.2 g, 58%) as a pale yellow solid.

1. customReaction mixture
2. temperaturewas cooled to 20-25° C
3. concentrationIt was then concentrated under vacuum
4. customquenched with cold water slowly
5. customsolid material was separated
6. filtrationIt was filtered off
7. washwashed with water
8. customThe solid material was dried under vacuum
9. customThe crude product was purified by column chromatography