反应详情

温度

160 °C

Under N2, methyl 2-chloro-6-methylisonicotinate (CAS 3998-90-1) (1.000 g, 5.39 mmol, Eq: 1.00), zinc cyanide (759 mg, 6.47 mmol, Eq: 1.2) and Tetrakis-triphenylphosphin-palladium (623 mg, 539 μmol, Eq: 0.1) were mixed in DMF (17 ml). The RM was stirred under microwave at 160° C. for 30 minutes. Control with TLC: the reaction was finished. The RM was partitioned between EtOAc and water; extracted; the organic phase was dried over MgSO4; filtered; concentrated in vacuo. The crude material was purified by flash chromatography (silica gel, 100 g, 5% to 30% EtOAc in heptane). Purple solid. MS (ISP): 177.2 ([M+H]+)

1. customThe RM was partitioned between EtOAc and water
2. extractionextracted
3. dry with materialthe organic phase was dried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe crude material was purified by flash chromatography (silica gel, 100 g, 5% to 30% EtOAc in heptane)