反应详情

To a stirred solution of sodium methoxide (257 mg. 4.8 mmol) in MeOH (20 mL) at room temperature was added 3-formyl-4-methoxyphenyl methyl carbonate (6, 1.0 g, 4.8 mmol). The resulting orange solution was stirred for 45 min and concentrated to dryness. The residue was dissolved in DMF (2 mL) and treated with K2CO3 (1.3 g, 9.4 mmol) and BnBr (0.57 mL, 4.8 mL). The reaction mixture was stirred for 15 h and it was poured into water (20 mL). The precipitate was collected, washed with water and dried in vacuo to afford the title compound (1.13 g, 98%) as a light yellow solid: 1H NMR (500 MHz, CDCl3) δ 10.44 (s, 1H), 7.49-7.41 (m, 3H), 7.40-7.36 (m, 2H), 7.35-7.30 (m, 1H), 7.21 (dd, J=9.1, 3.2 Hz, 1H), 6.95 (d, J=9.1 Hz, 1H), 5.05 (s, 2H), 3.90 (s, 3H); ESI MS m/z 243 [M+H]+.

1. concentrationconcentrated to dryness
2. dissolutionThe residue was dissolved in DMF (2 mL)
3. stirringThe reaction mixture was stirred for 15 h
4. customThe precipitate was collected
5. washwashed with water
6. customdried in vacuo