反应详情

温度

80 °C

Malononitril (15.0 g) was dissolved in dry DMF (200 mL). Subsequently, DBU (75 mL) and 1,5-dibromopentane (34 mL) were added at 0° C. (ice bath). The ice bath was removed and the reaction was stirred for 2 h at 80° C. After cooling down, the reaction was poured into DCM. The organic layer was washed several times with 5% NaHCO3, the organic layer dried over Na2SO4 and the solvent evaporated under reduced pressure. The crude product was purified by flash chromatography eluting with PA:EtOAc (9:1) yielding 25.7 g white crystals. 1H NMR (400 MHz, CDCl3) δ 1.48-1.61 (m, 2H), 1.68-1.84 (m, 4H), 2.13 (t, J=6 Hz, 4H).

1. customThe ice bath was removed
2. temperatureAfter cooling down
3. additionthe reaction was poured into DCM
4. washThe organic layer was washed several times with 5% NaHCO3
5. dry with materialthe organic layer dried over Na2SO4
6. customthe solvent evaporated under reduced pressure
7. customThe crude product was purified by flash chromatography
8. washeluting with PA