Ammonia → 3-[5-Fluoro-1-(2,3,6-trifluorobenzyl)-1H-pyrazolo[3,4-b]pyridin-3-yl]-7,7-dimethyl-5,7-dihydro-6H-pyrrolo[2,3-e][1,2,4]triazin-6-one

15 ml of phosphoryl chloride were added to 1.50 g (3.149 mmol) of the compound from Example 82A, and the mixture was stirred overnight. The reaction mixture was then taken up in 222 ml of acetonitrile and, with ice cooling, stirred into 133 ml of concentrated ammonia solution (33% in water). The reaction mixture was stirred at room temperature overnight and then concentrated on a rotary evaporator. Ethanol and water were added to the residue. A precipitate formed, which was filtered off and then washed with diethyl ether. Drying under high vacuum gave 982 mg of the title compound (70% of theory).

1. stirringThe reaction mixture was stirred at room temperature overnight
2. concentrationconcentrated on a rotary evaporator
3. additionEthanol and water were added to the residue
4. customA precipitate formed
5. filtrationwhich was filtered off
6. washwashed with diethyl ether
7. customDrying under high vacuum

ORD record

ord-ffb5d55c411248968044712179b6d014

Source dataset

uspto-grants-2015_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09216978B2