Triphosgene → 6-chloro-7-(morpholin-4-yl)-2H-1,2,4-triazolo[4,3-b]pyridazin-3-one

関与物質

反応手順

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+].

情報源と証拠