反应详情

温度

25 °C

To a solution of the title compound of Step A (3 mmol), and triethylamine (6 mmol) in CH2Cl2 (50 mL), was added MeSO3Cl (4 mmol). The mixture was stirred at 25° C. for 16 h. After concentration, ⅓ of the residue was dissolved in MeCN (20 mL). Next, 5-bromo-2-(3-fluoro-benzyloxy)-phenol (0.5 mmol) and K2CO3 (2 mmol) were added. The mixture was stirred at 100° C. for 16 h, concentrated and purified via PTLC providing the title compound (189 mg). MS (ESI): mass calcd. for C20H23BrFNO2, 407.1; m/z found, 408.0 [M+H]+. 1H NMR (CDCl3): 7.37-7.28 (m, 1H), 7.19-7.12 (m, 2H), 7.04-6.95 (m, 2H), 6.84-6.63 (m, 2H), 5.08 (s, 2H), 4.78-4.48 (m, 1H), 3.68-3.62 (m, 2H), 3.35-3.26 (m, 2H), 1.00 (s, 9H).

1. concentrationAfter concentration, ⅓ of the residue
2. dissolutionwas dissolved in MeCN (20 mL)
3. stirringThe mixture was stirred at 100° C. for 16 h
4. concentrationconcentrated
5. custompurified via PTLC