反应详情

温度

150 °C

A mixture of 1,3-dibromo-5-ethylbenzene (2.7 g, 10.2 mmol), copper cyanide (0.916 g, 10.2 mmol), pyridine (1.65 mL, 20.5 mmol) in DMF (15 mL) was heated at 150° C. for 3 h. After cooling to r.t., the mixture was poured into a solution of H2O (30 mL) and ammonia (25% aq. Solution, 20 mL) and extracted with EtOAc. The combined organic layer was dried (MgSO4), filtered and concentrated in vacuo. The product was purified using flash chromatography on silica gel, gradient elution of 0-60% EtOAc in n-heptane. GCMS (CI) m/z 210 [M+1]+.

1. temperatureAfter cooling to r.t.
2. extractionextracted with EtOAc
3. dry with materialThe combined organic layer was dried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe product was purified
7. washon silica gel, gradient elution of 0-60% EtOAc in n-heptane