反应详情

To a cold solution (0° C.) of 4-[3-[(E)-2-(3-dimethylaminomethyl-phenyl)-vinyl]-6-(4-hydroxy-phenyl)-1-(tetrahydro-pyran-2-yl)-1H-pyrazolo[3,4-b]pyridine-4-carbonyl]-piperazine-1-carboxylic acid tert-butyl ester (0.25 g, 0.37 mmol) in dry methanol (5 ml) was added dropwise a solution of aqueous 6N HCl (0.7 ml, 3.8 mmol). The reaction mixture was allowed to warm to room temperature and stirring was pursued for 2 hours before being concentrated under reduced pressure. Aqueous 6N HCl (0.7 ml, 3.8 mmol) was added to the crude mixture and stirring was pursued for another hour. Solvents were evaporated under vacuum, methanol and diethyl ether were added, the resulting precipitate was filtered and dried to give a chlorhydrate salt of the title compound as an orange solid (0.21 g; 95%).

1. concentrationbefore being concentrated under reduced pressure
2. stirringstirring
3. waitwas pursued for another hour
4. customSolvents were evaporated under vacuum, methanol and diethyl ether
5. additionwere added
6. filtrationthe resulting precipitate was filtered
7. customdried