反应详情

A mixture of 3,6-dichloro-4-(3,6-dihydro-2H-pyridin-1-yl)pyridazine (1.7 g, 7.4 mmol) and hydrazine hydrate (2.2 ml) in dioxan was stirred and heated at reflux under nitrogen for 24 hours. Upon cooling the dioxan was removed in vacuo and the residue was partitioned between dichloromethane and water. The aqueous was further extracted with dichloromethane (×3). The combined extracts were dried (MgSO4), filtered and evaporated. The residue was triturated with ether/MeOH and dried in vacuo to afford the title pyridazine (1.5 g, 88%). 1H NMR (250 MHz, d6-DMSO) 7.8 (1H, br s), 6.48 (1H, s), 5.76 (2H, m), 4.21 (2H, br s), 3.51 (2H, m), 3.24 (2H, m), 2.16 (2H, m). MS (ES+) 226 [MH]+, 228 [MH]+.

1. temperatureheated
2. temperatureat reflux under nitrogen for 24 hours
3. customwas removed in vacuo
4. customthe residue was partitioned between dichloromethane and water
5. extractionThe aqueous was further extracted with dichloromethane (×3)
6. dry with materialThe combined extracts were dried (MgSO4)
7. filtrationfiltered
8. customevaporated
9. customThe residue was triturated with ether/MeOH
10. customdried in vacuo