Dimethyl 2,2-dimethyl-3-oxobutanedioate → HCID 178500130, compound

Participants

Reaction Steps

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).

Provenance & Evidence