反应详情

218 mg (1.13 mmol) of dimethyl 2,2-dimethyl-3-oxobutanedioate were initially charged in 5 ml of ethanol and heated to reflux. Subsequently, 205 mg (0.75 mmol) of 1-(2-fluorobenzyl)-1,4,5,6-tetrahydrocyclopenta[c]pyrazole-3-carboximidohydrazide suspended in 5 ml of ethanol were added and the mixture was boiled under reflux overnight. After cooling, the mixture was filtered, the filtercake was washed with a little ethanol and the filtrate was concentrated. The residue was purified by means of preparative HPLC (eluent: acetonitrile/water, gradient 20:80→100:0). 48 mg of the target compound were obtained (purity 54%; 8% of theory).

1. temperatureheated to reflux
2. additionwere added
3. temperatureunder reflux overnight
4. temperatureAfter cooling
5. filtrationthe mixture was filtered
6. washthe filtercake was washed with a little ethanol
7. concentrationthe filtrate was concentrated
8. customThe residue was purified by means of preparative HPLC (eluent: acetonitrile/water, gradient 20:80→100:0)