反应详情

温度

160 °C

A solution of C-[3-(4-fluoro-phenyl)-5-methyl-isoxazol-4-yl]-methylamine (206 mg, 1.0 mmol) and 3,6-dichloropyridazine (149 mg, 1.0 mmol) in DMSO (2 mL) containing N,N-diisopropyl ethyl amine (259 mg, 342 μL, 2.0 mmol) was heated with microwave irradiation to 160° C. for 1 h. After cooling to room temperature the reaction mixture was extracted (ethyl acetate/water). The organic phase was dried over sodium sulfate and concentrated. Purification by chromatography (SiO2, heptane:ethyl acetate=100:0 to 1:1) afforded the title compound (99 mg, 31%) as an off white solid after recrystallization from heptane:ethyl acetate. MS: m/e=319.1 [M+H]−.

1. temperatureAfter cooling to room temperature the reaction mixture
2. extractionwas extracted (ethyl acetate/water)
3. dry with materialThe organic phase was dried over sodium sulfate
4. concentrationconcentrated
5. customPurification by chromatography (SiO2, heptane:ethyl acetate=100:0 to 1:1)