反应详情

Triphosgene (750 mg, 2.5 mmol) was added to a stirred solution of 6-chloro-5-(morpholin-4-yl)pyridazin-3-ylhydrazine (1.42 g, 6.2 mmol) in 1,2-dichloroethane (60 ml) at room temperature under nitrogen. The mixture was then stirred and heated at reflux for 22 hours. Upon cooling the precipitate was collected by filtration. The solid was washed with diethyl ether anid then dried in vacuo to give 6-chloro-7-(morpholin-4-yl)-2 H-1,2,4-triazolo[4,3-b]pyridazin-3-one (1.1 g, 67%) which was used without further purification. Data for the title compound: 1H NMR (250 MHz, d6-DMSO) δ3.02-3.05 (4 H, m), 3.72-3.76 (4 H, m), 7.19 (1 H, s), 12.57 (1 H, br s); MS (ES+) m/e 256, 258 [MH+].

1. temperatureheated
2. temperatureat reflux for 22 hours
3. temperatureUpon cooling the precipitate
4. filtrationwas collected by filtration
5. washThe solid was washed with diethyl ether
6. customdried in vacuo