反应详情

A solution of KCN (3.8 g, 58 mmol) was stirred in DMF (150 mL) at room temperature. After the mixture was stirred for 2 h, a solution of 2-ethylhexylbromide (10 g, 52 mmol) in DMF (250 mL) was added dropwise at the same temperature. After stirring for 12 h at room temperature, the reaction mixture was concentrated by evaporation in vacuo. The crude product was diluted with water (100 mL) and diethyl ether (100 mL). The organic layer was separated and the aqueous layer was extracted with diethyl ether. The combined organic layers were subsequently washed with NaOH-solution (2.5 M), saturated bicarbonate solution and brine, dried over MgSO4 and concentrated by evaporation in vacuo. The resulting brown oil was purified by vacuum distillation (45° C., 10−2 mbar) to afford a clearly yellow oil (VI). (3.2 g, 44%). 1H-NMR (CDCl3): δ=2.82-2.69 (m, 2H), 2.22-2.15 (m, 1H), 1.55-1.00 (m, 11H), 0.83-0.68 (m, 3H)

1. stirringAfter stirring for 12 h at room temperature
2. concentrationthe reaction mixture was concentrated by evaporation in vacuo
3. additionThe crude product was diluted with water (100 mL) and diethyl ether (100 mL)
4. customThe organic layer was separated
5. extractionthe aqueous layer was extracted with diethyl ether
6. washThe combined organic layers were subsequently washed with NaOH-solution (2.5 M), saturated bicarbonate solution and brine
7. dry with materialdried over MgSO4
8. concentrationconcentrated by evaporation in vacuo
9. distillationThe resulting brown oil was purified by vacuum distillation (45° C., 10−2 mbar)