Dimethylformamide → HCID 14986975, compound

Participants

Reaction Steps

To 50 ml of dry dimethylformamide is added 4.5 g of 2-(4-chlorophenyl)-9-hydroxy-2,3,4,4a-tetrahydro-5H-(1)benzothiopyrano[4,3-c]pyridazin-3-one, and 0.7 g of 60% sodium hydride is added thereto while stirring at room temperature. After stirring at room temperature for 1 hour and addition of 2 g of 3-dimethylaminopropyl chloride, the mixture is stirred under heating at 40°-50° C. for 3 hours. After the completion of the reaction, the reaction mixture is poured into a large amount of water and the mixture is extracted with chloroform. The extract is washed with water and dried over anhydrous magnesium sulfate. Thereafter, the solvent is distilled off. The residue is subjected to column chromatography and the eluate is converted into its fumarate to give 0.52 g of 2-(4-chlorophenyl)-9-(3-dimethylaminopropoxy)-2,3,4,4a-tetrahydro-5H-(1)benzothiopyrano[4,3-c]pyridazin-3-one.fumarate, as yellow crystals, m.p. 208°-210° C.

Provenance & Evidence