反应详情

841 mg (4.473 mmol) of dimethyl 2,2-dimethyl-3-oxobutanedioate were initially charged in 20 ml of ethanol, and the mixture was heated to reflux. Subsequently, 1.070 g (2.982 mmol) of 1-(cyclopentylmethyl)-5-fluoro-1H-pyrazolo[3,4-b]pyridine-3-carboximidohydrazide suspended in 26 ml of ethanol were added, and the mixture was boiled under reflux overnight. After cooling, the mixture was concentrated, taken up in acetonitrile and filtered. The filtrate was purified by preparative HPLC (mobile phase: acetonitrile/water, gradient 30:70→100:0). This gave 396 mg of the target compound (32% of theory).

1. temperaturethe mixture was heated to reflux
2. additionwere added
3. temperatureunder reflux overnight
4. temperatureAfter cooling
5. concentrationthe mixture was concentrated
6. filtrationfiltered
7. customThe filtrate was purified by preparative HPLC (mobile phase: acetonitrile/water, gradient 30:70→100:0)