HCID 14726219, compound → HCID 14726454, compound

Participants

Reaction Steps

4.25 g (0.0093 mol) of 2-t-butyl-5-chloro-4-((2(4-(3-trifluoromethylphenyl)-1-piperazinyl)ethyl)amino)-3(2H)-pyridazinone are stirred with 50 ml of concentrated aqueous hydrochloric acid at room temperature for 72 hours, made basic and extracted 3 times with chloroform, 10 the organic phase is concentrated and dried with sodium sulphate, and the residue is triturated with acetone. The crystalline precipitate of 5-chloro-4-((2-(4-(3-trifluoromethylphenyl)-1-piperazinyl)ethyl)amino)-3(2H)-pyridazinone weighs 2.40 g (47.7% of theory). It is converted by dissolving in 100 ml of hot absolute ethanol and adding ethereal hydrochloric acid into 2.20 g (46.7% of theory) of dihydrochloride of m.p. 220°-223° C.; C 40.6%, H 4.2%, Cl(tot) 21.1%, Cl- 14.2%, F 11.5%, N 13.9%, O 8.7%, UV in 0.1N HCl: 208(4.42), 226(S,4.22), 300(4.47).

Provenance & Evidence