反应详情

A mixture of methyl 4-({[1,6-diethyl-4-(tetrahydro-2H-pyran-4-ylamino)-1H-pyrazolo[3,4-b]pyridin-5-yl]methyl}amino)-4-oxobutanoate (520 mg, 1.25 mmol), LiOH (261 mg, 6.23 mmol), water (3 mL) and methanol (6 mL) was stirred at room temperature overnight. The aqueous layer was acidified with 2 N HCl to PH<1. Brine (30 mL) was added to the solution. The aqueous layer was extracted with a mixture of DCM:IPA (4:1) twice. The combined organic layers were dried over sodium sulfate, filtered and then concentrated under vacuum to give 4-({[1,6-diethyl-4-(tetrahydro-2H-pyran-4-ylamino)-1H-pyrazolo[3,4-b]pyridin-5-yl]methyl}amino)-4-oxobutanoic acid as a white solid (350 mg, 70%): LC-MS m/z 404 (M+H)+.

1. extractionThe aqueous layer was extracted with a mixture of DCM:IPA (4:1) twice
2. dry with materialThe combined organic layers were dried over sodium sulfate
3. filtrationfiltered
4. concentrationconcentrated under vacuum