反应详情

In 40 ml of dry dimethylformamide (DMF) was dissolved 8.13 g of 6-(p-aminophenyl)-5-methyl-4,5-dihydro-3(2H)-pyridazinone. To this solution was added 3.5 g of methyl thioisocyanate, and the mixture was stirred for 4 hours at room temperature. The mixture was stirred for an additional 30 minutes at 50° C. and the solvent was distilled off under reduced pressure. To the residue was added 50 ml of dichloromethane/ether (1:1) to precipitate crystals which were then collected by filtration and washed with dichloromethane, whereby 10.1 g of the above-identified compound was obtained. M.P. 213° C.

1. stirringThe mixture was stirred for an additional 30 minutes at 50° C.
2. distillationthe solvent was distilled off under reduced pressure
3. additionTo the residue was added 50 ml of dichloromethane/ether (1:1)
4. customto precipitate crystals which
5. filtrationwere then collected by filtration
6. washwashed with dichloromethane