反应详情

A mixture of 75 (1.50 g, 5.08 mmol) and AlCl3 (3.50 g, 26.2 mmol) were refluxed in benzene (50 mL) for 3 h and then cooled to RT. Water (100 mL) was cautiously added dropwise, and the mixture was extracted with Et2O (3×100 mL). The combined ethereal extracts were washed with water (200 mL), brine (200 mL), and dried over MgSO4. Concentration afforded 1.39 g (97%) of 76 that was used without further purification. 1H NMR (400 MHz, CDCl3): δ 5.73 (br s, 1H), 6.90 (d, J=8.8 Hz, 2H), 7.35-7.41 (m, 3H), 7.77 (d, J=8.4 Hz, 2H).

1. extractionthe mixture was extracted with Et2O (3×100 mL)
2. washThe combined ethereal extracts were washed with water (200 mL), brine (200 mL)
3. dry with materialdried over MgSO4
4. concentrationConcentration