反应详情

50.000 g (163.535 mmol) of 1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridine-3-carboximidamide hydrochloride were dissolved in 700 ml of ethanol, and 66.192 g (654.141 mmol) of triethylamine and 10.233 g (163.535 mmol) of hydrazine hydrate (80% strength solution in water) were added at 0° C. The mixture was stirred at RT overnight and then concentrated on a rotary evaporator. The residue was taken up in ethyl acetate and the solution was washed three times with saturated aqueous sodium chloride solution. The organic phase was dried over sodium sulphate and concentrated on a rotary evaporator. The residue was stirred with diethyl ether, filtered off with suction and dried under high vacuum. 46.49 g (46% of theory, 68% pure) of the title compound were obtained.

1. concentrationconcentrated on a rotary evaporator
2. washthe solution was washed three times with saturated aqueous sodium chloride solution
3. dry with materialThe organic phase was dried over sodium sulphate
4. concentrationconcentrated on a rotary evaporator
5. stirringThe residue was stirred with diethyl ether
6. filtrationfiltered off with suction
7. customdried under high vacuum