反应详情

A mixture of 4.5 (0.15 mmol), 6-(bromomethyl)-1,1,4,4-tetramethyl-1,2,3,4-tetrahydronaphthalene (0.18 mmol) and cesium carbonate (0.2 mmol) in DMF (2 mL), was stirred at room temperature for 16 hours. To the reaction mixture was added LiOH in water (1 mL, 1N solution), and the reaction was stirred at 50° C. for 3 hours. The mixture was filtered and purified by reverse phase HPLC to give 4 (35 mg, 0.08 mmol) after lyophilization. MS ESI (pos.) m/e 447.3 (M+H). 1H NMR (500 MHz) (CDCl3) δ 8.64 (1 H, s), 7.59 (1 H, s), 7.33-7.36 (2 H, m), 7.20 (1 H, dd, J=7.9, 1.8 Hz), 7.08 (2 H, d, J=8.5 Hz), 6.98 (2 H, d, J=8.5 Hz), 4.98 (2 H, s), 4.53 (1 H, m), 3.57 (3 H, s), 2.96-3.06 (2 H, m), 1.71 (4 H, s), 1.31 (6 H, s), 1.30 (6 H, s).

1. stirringthe reaction was stirred at 50° C. for 3 hours
2. filtrationThe mixture was filtered
3. custompurified by reverse phase HPLC