反应详情

0.66 ml of a 2N solution of hydrogen chloride in diethyl ether was added to 81 mg (0.13 mmol; purity 91%) of tert.-butyl-(1-[2-[1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridin-3-yl]-5,5-dimethyl-6-oxo-6,7-dihydro-5H-pyrrolo[2,3-d]pyrimidin-4-yl]azetidin-3-yl)carbamate (example 62A) and it was stirred for 4 h at room temperature. The reaction solution was concentrated by evaporation and purified twice by preparative HPLC (acetonitrile/water (+0.1% trifluoroacetic acid) gradient). The concentrated fractions were dissolved in dichloromethane and washed twice with saturated aqueous sodium hydrogen carbonate solution. The combined aqueous phases were extracted twice with dichloromethane. The combined organic phases were dried over sodium sulphate, filtered and concentrated by evaporation. 31 mg (49% of theor.) of the target compound was obtained.

1. concentrationThe reaction solution was concentrated by evaporation
2. custompurified twice by preparative HPLC (acetonitrile/water (+0.1% trifluoroacetic acid) gradient)
3. dissolutionThe concentrated fractions were dissolved in dichloromethane
4. washwashed twice with saturated aqueous sodium hydrogen carbonate solution
5. extractionThe combined aqueous phases were extracted twice with dichloromethane
6. dry with materialThe combined organic phases were dried over sodium sulphate
7. filtrationfiltered
8. concentrationconcentrated by evaporation
9. custom31 mg (49% of theor.) of the target compound was obtained