Dimethylamine → HCID 178484499, compound

Participants

Reaction Steps

di(imidazol-1-yl)methanone (1910 mg) was added portionwise to a suspension of 4-bromo-1H-pyrazole-3-carboxylic acid (900 mg) in DCM (18 ml).After 2 hours dimethylamine 2M in THF (9.42 ml) was added portionwise and the mixture was stirred overnight. The reaction mixture was purified by preparative HPLC using a Waters X-Bridge reverse-phase column (5 microns silica, 30 mm diameter, 150 mm length) and decreasingly polar mixtures of water (containing 0.2% ammonium carbonate) and acetonitrile as eluent. The fractions were evaporated to dryness to afford 4-bromo-N,N-dimethyl-1H-pyrazole-3-carboxamide (471 mg) as a solid. NMR Spectrum: (DMSOd6): 2.95 (s, 3H), 2.98 (s, 3H), 7.99 (s, 1H); Mass spectrum: M+H+ 220.

Provenance & Evidence