反应详情

温度

0 °C

To 11H-benzo[a]carbazole (0.70 g; 3.22 mmol) in DMF (3 ml) is added sodium hydride (0.19 g; 4.67 mmol) at 0° C., After stirring 1 h at 0° C., 1-bromo-2-ethylhexane (1.24 g; 6.44 mmol) is added at 0° C., and the mixture is stirred at room temperature overnight. The reaction mixture is poured into ice-water, and the crude product is extracted twice with AcOEt (acetic acid ethyl ester). The combined organic layer is washed with H2O and brine, dried over MgSO4, and concentrated and dried in vacuo to give a yellow liquid as a crude product (1.08 g). The product is used for the next reaction without further purification. The structure is confirmed by 1H-NMR spectrum (CDCl3). δ [ppm]: 0.80-0.92 (m, 6H), 1.16-1.47 (m, 8H), 2.27 (m, 1H), 4.65-4.69 (m, 2H), 7.27 (td, 1H), 7.44-7.59 (m, 4H), 7.66 (d, 1H), 8.02 (d, 1H), 8.14 (d, 1H), 8.18 (d, 1H), 8.54 (d, 1H).

1. stirringthe mixture is stirred at room temperature overnight
2. extractionthe crude product is extracted twice with AcOEt (acetic acid ethyl ester)
3. washThe combined organic layer is washed with H2O and brine
4. dry with materialdried over MgSO4
5. concentrationconcentrated
6. customdried in vacuo