Ethanol → HCID 90011519, compound

Participants

Reaction Conditions

Reaction Steps

Step-3: 1-(5-Bromopyridin-2-yl)-N-hydroxy-5-(trifluoromethyl)-1H-pyrazole-3-carboximidamide: A mixture of step-2 intermediate (150 mg, 0.473 mmol), hydroxylamine hydrochloride (82 mg, 1.183 mmol) and Na2CO3 (125 mg, 1.183 mmol) in ethanol (10 mL) was stirred at 85° C. for 6 h. Reaction mixture was cooled to room temperature and the solvent was evaporated under vacuum. Water (10 mL) was added to the obtained residue and extracted with ethyl acetate (2×25 mL). The combined organic layers were washed with water (20 mL), brine (20 mL), dried (Na2SO4) and filtered. The filtrate was concentrated under vacuum to afford 106 mg (64%) of the title compound as a white solid. 1HNMR (400 MHz, DMSO- d6) δ 9.96 (s, 1H), 8.69 (d, J=2.0 Hz, 1H), 8.37 (dd, J=2.0 & 8.0 Hz, 1H), 8.00 (d, J=8.0 Hz, 1H), 7.23 (s, 1H), 5.93 (s, 2H); ESI-MS (m/z) 350, 352 [(MH)+, Br79,81].

Provenance & Evidence