反应详情

22.000 g (purity 68%, approx. 52.621 mmol) of 1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridine-3-carboximidohydrazide in 220 ml of ethanol were initially introduced, admixed dropwise with 18.265 (89.455 mmol) of ethyl oxoacetate (50% strength solution in toluene) and heated under reflux overnight. The resulting suspension was concentrated on a rotary evaporator and stirred with diethyl ether. The solid was filtered off with suction and dried under high vacuum. Further purification was effected by chromatography on silica gel (mobile phase: dichloromethane/methanol, gradient 30:1→10:1). This gave 12.07 g of the target compound (purity 69%; 49% of theory).

1. temperatureheated
2. temperatureunder reflux overnight
3. concentrationThe resulting suspension was concentrated on a rotary evaporator
4. filtrationThe solid was filtered off with suction
5. customdried under high vacuum
6. customFurther purification