反应详情

温度

115 °C

A mixture of 2,5-dibromo-3-methylpyridine (20.17 g, 80.4 mmol) and copper(I) cyanide (7.24 g, 80.8 mmol) in 200 mL DMF was heated to 115° C. overnight. The reaction mixture was cooled to 25° C. and poured into 600 mL of H2O. The solid was filtered, washed with copious amounts of H2O. The filtrate was extracted with EtOAc (4×) and the combined organic layers were washed with H2O and dried over Na2SO4. The solution was filtered, evaporated onto silica gel and purified by flash chromatography eluting with EtOAc:hexane (0:1→1:9) to give the title compound as a white solid. MS m/z: 197.0 [M+1].

1. temperatureThe reaction mixture was cooled to 25° C.
2. filtrationThe solid was filtered
3. washwashed with copious amounts of H2O
4. extractionThe filtrate was extracted with EtOAc (4×)
5. washthe combined organic layers were washed with H2O
6. dry with materialdried over Na2SO4
7. filtrationThe solution was filtered
8. customevaporated onto silica gel
9. custompurified by flash chromatography
10. washeluting with EtOAc:hexane (0:1→1:9)