反应详情

3 ml tert.-butanol, a solution of 146 mg (0.70 mmol) of methyl-3,3-dicyano-2,2-dimethylpropanoate in 1.5 ml tert.-butanol and 94 mg (0.84 mmol) of potassium tert.-butylate were added to 200 mg (0.70 mmol) of 1-(2-fluorobenzyl)-6-methyl-1H-pyrazolo[3,4-d]pyrimidine-3-carboximidamide and it was heated under reflux for 48 h. Water was added and the precipitate was filtered off. The filtrate was extracted with dichloromethane, the organic phase was dried over sodium sulphate and concentrated in a rotary evaporator. The residue was mixed with water/ethanol. The solid was filtered off and dried under high vacuum. 102 mg (34% of theor.) of the target compound was obtained.

1. temperaturewas heated
2. temperatureunder reflux for 48 h
3. filtrationthe precipitate was filtered off
4. extractionThe filtrate was extracted with dichloromethane
5. dry with materialthe organic phase was dried over sodium sulphate
6. concentrationconcentrated in a rotary evaporator
7. additionThe residue was mixed with water/ethanol
8. filtrationThe solid was filtered off
9. customdried under high vacuum
10. custom102 mg (34% of theor.) of the target compound was obtained