Hydrochloric Acid → HCID 15079112, compound

Participants

Reaction Conditions

Reaction Steps

A mixture comprising 256 mg of 2-(2-trimethylsilylethoxymethyl)-4-chloro-5-(3,4-dimethoxybenzylamino)-6-n-propylmercapto-3(2H)pyridazinone prepared in Reference Example 5, 3 ml of tetra-n-butylammonium fluoride (1M tetrahydrofuran solution) and 1.5 ml of N,N-dimethylformamide, was stirred at a temperature of 150° C. for 3 hours. A 1N hydrochloric acid aqueous solution was added to the reaction mixture, and the mixture was extracted with chloroform. The extract was washed with water and a sodium hydrogencarbonate aqueous solution in this order, and dried over sodium sulfate. The solvent was distilled off and the residue thereby obtained was purified by silica gel thin layer chromatography by using benzene-ethyl acetate (1:1 v/v) as the developer, to obtain 39 mg of the above identified compound as a light yellow solid substance. The product was changed into slightly yellow crystals having a melting point of from 129° to 130° C. by the recrystallization thereof from a solvent mixture of ethyl acetate-diethyl ether-n-hexane.

Provenance & Evidence