Toluene → 3-bromo-N-(4-chloro-2-(1-cyclopropylethylcarbamoyl)phenyl)-1-(3-chloropyridin-2-yl)-4,5-dihydro-1H-pyrazole-5-carboxamide

Participants

Reaction Conditions

Reaction Steps

0.25 g of calcium bromide dihydrate was added to a mixed liquid comprising 1.0 g of 5-(4-chloro-2-(1-cyclopropylethylcarbamoyl)phenylcarbamoyl)-1-(3-chloropyridin-2-yl)-4,5-dihydro-1H-pyrazol-3-yl 4-methylbenzenesulfonate and 10 ml of toluene, followed by heating at about 90° C. for 6.5 hours. After the reaction liquid was stood to cool, 0.41 g of sodium hydrogen carbonate and 10 ml of water were added to the reaction liquid, followed by stirring. After liquid-liquid separation, the organic layer was washed with a saturated sodium chloride aqueous solution and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to obtain 0.96 g of the crude desired product.

Provenance & Evidence