Sodium Bicarbonate → HCID 11271378, compound

Participants

Reaction Conditions

Reaction Steps

8-(4-Bromo-2,6-dimethyl-phenyl)-2-methyl-4-(1-propyl-butylamino)-pyrrolo[1,2-a]pyrimidine-6-carbonitrile (10.0 g) was added into conc. H2SO4 (50 mL) and heated for 55° C. for 5 hours. The reaction mixture was cooled to room temperature, poured into ice-water and then a saturated aqueous sodium hydrogencarbonate was added to make the aqueous mixture alkaline (pH=8) and extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated under reduced pressure and the residue was purified by a silica gel column chromatography (silica gel: Wako Gel (C200), eluent: hexane/ethyl acetate/chloroform=10:3:1) to give a solid. The solid was recrystallized from ethyl acetate to provide 8-(4-bromo-2,6-dimethyl-phenyl)-2-methyl-4-(1-propyl-butylamino)-pyrrolo[1,2-a]pyrimidine-6-carboxylic acid amide (5.8 g).

Provenance & Evidence