反应详情

To 11H-benzo[a]carbazole (1.06 g, 3.23 mmol) in CH2Cl2 (5 ml) are added AlCl3 (0.510 g, 3.82 mmol) and 2,4,6-trimethylbenzoyl chloride (0.59 g, 3.24 mmol) at 0° C. After stirring at room temperature for 1 hour, AlCl3 (0.51 g, 3.82 mmol) and phenylacetyl chloride (0.52 g, 3.39 mmol) are added at 0° C. The reaction mixture is stirred at room temperature for 2 hours, and then it is poured into ice-water. The crude product is extracted with CH2Cl2, and washed with water and brine. After drying over MgSO4 and concentration, the product is reprecipitated from CH2Cl2 and n-hexane to obtain a white powder (1.53 g, 81%). The structure is confirmed by 1H-NMR spectrum (CDCl3). δ [ppm]: 0.79-0.91 (m), 1.18-1.50 (m), 2.19 (s), 2.28 (m), 2.41 (s), 4.38 (s), 4.74 (m), 6.97 (s), 7.22-7.36 (m), 7.56 (d), 7.71 (t), 7.77 (t), 8.14 (d), 8.35 (s), 8.62 (d), 8.63 (s), 9.58 (s).

1. stirringThe reaction mixture is stirred at room temperature for 2 hours
2. extractionThe crude product is extracted with CH2Cl2
3. washwashed with water and brine
4. dry with materialAfter drying over MgSO4 and concentration
5. customthe product is reprecipitated from CH2Cl2 and n-hexane