Compound2(6.0 g, 9.010 3 mol) was dissolved in anhydrous THF (100 mL) andn-butyllithium (2.2 M/hexane, 6 mL, 0.0132 mol) was added, dropwise, under an argon atomosphere at 78 C. After stirring for 5 h, B(OCH3)3 (2.2 mL) was added quickly at78 C and the mixture was stirred overnight allowing the temperature to rise gradually to room temperature. Then, the reaction mixture was acidified with hydrochloric acid (2 M) for 2 h. The mixture was extracted with dichloromethane (3 50 mL) and the organic layer was dried with anhydrous sodium sulfate. After removing the solvent under reduced pressure, the crude product was purified by silica gel column chromatography using acetone/CH2Cl2 (1 : 20, v) as eluent to yield 3(2.1 g, yield 55%). 1 H-NMR (300 MHz, DMSO-d6) d: 7.137 (s, 1H, >C]CH–), 7.25–7.58 (m, 16 H), 7.62–7.78 (m, 8 H), 7.976 (s, 2 H, –B(OH)2), 8.20–8.30 (m, 4 H, carbazole–H); MS (EI),m/ z: 586 ([M-(B(OH)2)] + , calcd for C44H29, 585); anal. calc. For C44H31BN2O2: C 83.81, H 4.96, N 4.44; found: C 83.64, H 4.89,
N 4.48. |
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