反应详情

温度

150 °C

To a solution of 2-ethoxy-6-iodo-3-methoxypyridine (16-2, 100 mg, 0.36 mmol, 1 equiv) in DMF (675 uL) was added copper cyanide (39 mg, 0.43, mmol, 1.2 equiv). The reaction mixture was heated in a microwave reactor at 150° C. for 20 minutes, and then was partitioned between DCM (50mL) and water (50 mL). The aqueous layer was extracted with DCM (3×25 mL), and the organic phase was dried over Mg2SO4, concentrated and purified by normal phase column chromatography (20-50% EtOAc in hexanes) to yield the title compound (16-3) as a white solid. ESI+MS [M+H]+ C9H11N2O2: 179.1 found, 179.2 required.

1. customwas partitioned between DCM (50mL) and water (50 mL)
2. extractionThe aqueous layer was extracted with DCM (3×25 mL)
3. dry with materialthe organic phase was dried over Mg2SO4
4. concentrationconcentrated
5. custompurified by normal phase column chromatography (20-50% EtOAc in hexanes)