反应详情

374 mg (1.985 mmol) of dimethyl 2,2-dimethyl-3-oxobutanedioate were initially charged in 8 ml of ethanol and heated to reflux. Subsequently, 420 mg (1.324 mmol) of 1-(2,3-difluorobenzyl)-6-methyl-1H-pyrazolo[3,4-d]pyrimidine-3-carboximidohydrazide suspended in 8 ml of ethanol were added and the mixture was heated to reflux overnight. Another 299 mg (1.588 mmol) of dimethyl 2,2-dimethyl-3-oxobutanedioate dissolved in 3 ml of ethanol were added and the mixture was boiled under reflux overnight. After cooling, the mixture was filtered and purified directly by means of preparative HPLC (eluent: acetonitrile/water, gradient 30:70→100:0). 163 mg of the target compound were obtained (purity 89%; 24% of theory).

1. temperatureheated to reflux
2. additionwere added
3. temperaturethe mixture was heated
4. temperatureto reflux overnight
5. additionwere added
6. temperatureunder reflux overnight
7. temperatureAfter cooling
8. filtrationthe mixture was filtered
9. custompurified directly by means of preparative HPLC (eluent: acetonitrile/water, gradient 30:70→100:0)