反应详情

温度

50 °C

To a suspension of 3-chloro-6-[3-(4-fluoro-phenyl)-5-methyl-3H-[1,2,3]triazol-4-ylmethoxy]-pyridazine (696 mg, 2.18 mmol) in ethanol (11 mL) was added sodium carbonate (231 mg, 2.18 mmol) followed by 1,1′-bis(diphenylphosphino) ferrocene (121 mg, 0.22 mmol) and palladium(II) acetate (49 mg, 0.22 mmol). The reaction flask was filled with Ar three times after a short evacuation. The fourth time the flask was flushed with CO-gas (balloon). The mixture was stirred under CO atmosphere at 50° C. over night, then cooled to room temperature and filtered over dicalite and washed well with DCM. The filtrate was then evaporated. Purification by chromatography (silica, 0 to 50% ethyl acetate in heptane) afforded the title compound (725 mg, 93%) as a light yellow gum. MS: m/e=358.2 [M+H]+.

1. additionThe reaction flask was filled with Ar three times after a short evacuation
2. customThe fourth time the flask was flushed with CO-gas (balloon)
3. temperaturecooled to room temperature
4. filtrationfiltered over dicalite
5. washwashed well with DCM
6. customThe filtrate was then evaporated
7. customPurification by chromatography (silica, 0 to 50% ethyl acetate in heptane)