反应详情

温度

50 °C

To a suspension of 3-chloro-6-(3-methyl-5-pyridin-2-yl-3H-[1,2,3]triazol-4-ylmethoxy)-pyridazine (620 mg, 2.05 mmol) in ethanol (10 mL) was added sodium carbonate (220 mg, 2.05 mmol) followed by 1,1′-bis(diphenylphosphino) ferrocene (115 mg, 0.21 mmol) and palladium(II) acetate (46 mg, 0.21 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 (582 mg, 84%) as an off white solid. MS: m/e=341.1 [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)