反应详情

160 mg (purity 89%, 0.313 mmol) of methyl 2-{3-[1-(2,3-difluorobenzyl)-6-methyl-1H-pyrazolo[3,4-d]pyrimidin-3-yl]-5-hydroxy-1,2,4-triazin-6-yl}-2-methylpropanoate were admixed with 4 ml (42.913 mmol) of phosphoryl chloride and the mixture was stirred at RT for 2.5 h. The reaction solution was diluted with 20 ml of dry acetonitrile and gradually added dropwise while cooling with ice to 40 ml of a 25% aqueous ammonia solution, and the mixture was stirred at RT for 1 h. The reaction mixture was concentrated on a rotary evaporator and the precipitate was filtered off. The residue was stirred with hot ethanol/water and filtered with suction, and the solids were dried under high vacuum. 70 mg of the target compound were obtained (52% of theory).

1. additiongradually added dropwise
2. stirringthe mixture was stirred at RT for 1 h
3. concentrationThe reaction mixture was concentrated on a rotary evaporator
4. filtrationthe precipitate was filtered off
5. stirringThe residue was stirred with hot ethanol/water
6. filtrationfiltered with suction
7. customthe solids were dried under high vacuum