反应详情

温度

160 °C

2,3,6-Trifluorobenzoyl chloride (4.0 g) was added dropwise to a cooled (15° C.) solution of 3-chloro-4-(1,1-dimethylethyl)-6-hydrazinylpyridazine (4 g) in dry 1-methyl-2-pyrrolidinone (50 ml). After the addition the reaction mixture was heated at 160° C. for 24 h. The reaction mixture was cooled to room temperature, diluted with ethyl acetate (200 ml), and washed twice with water (200 ml). The organic phase was separated, dried (sodium sulfate), and evaporated at reduced pressure. The residue was crystallised from dichloromethane on dilution with diethyl ether to afford the title compound (5.3 g) as a colourless solid: 1H NMR (400 MHz, DMSO-d6) δ1.52 (9H, s), 7.50 (1H, m), 7.92 (1H, m), 8.45 (1H, s); MS (ES30) m/z 341/343 [MH]+.

1. additionAfter the addition the reaction mixture
2. temperatureThe reaction mixture was cooled to room temperature
3. washwashed twice with water (200 ml)
4. customThe organic phase was separated
5. dry with materialdried (sodium sulfate)
6. customevaporated at reduced pressure
7. customThe residue was crystallised from dichloromethane on dilution with diethyl ether