Ammonium Hydroxide → HCID 21929458, compound

Participants

Reaction Conditions

Reaction Steps

0.718 g of 1-hydroxybenzotriazole hydrate and 1.27 g of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride are added to 1.4 g of 6,6-diphenyl-6,7-dihydro-1H-indazole-3-carboxylic acid in suspension in 200 cm3 of chloroform. After stirring for 30 minutes at a temperature in the region of 20° C., 1.5 cm3 of aqueous 28% ammonium hydroxide solution are added dropwise to the reaction mixture. After stirring at a temperature in the region of 20° C. for about 20 hours, the reaction mixture is diluted with 300 cm3 of chloroform and washed with three times 100 cm3 of water. The organic phases are dried over magnesium sulphate, filtered and concentrated to dryness under reduced pressure (13 kPa). The solid is taken up in 10 cm3 of dichloromethane, cooled to a temperature in the region of 5° C., drained by suction, washed with three times 5 cm3 of diisopropyl ether and dried over potassium hydroxide under reduced pressure (13 kPa), at a temperature in the region of 20° C. 1.2 g of 6,6-diphenyl-6,7-dihydro-1H-indazole-3-carboxamide are thus obtained in the form of a cream-coloured powder, the characteristics of which are as follows:

Provenance & Evidence