反应详情

(39) To a solution of 2,6-dimethoxybenzaldehyde (250 mg, 1.50 mmol) and acetophenone (180 mg, 1.50 mmol) in 2.2 ml of methanol was added 1.0 ml of 40% sodium hydroxide in water at 10° C. After stirring overnight at room temperature, a solid precipitated. The precipitate was recrystallized from methanol to afford 350 mg (87.1%) of a white, flaky solid: mp 54.9-55.8° C. (lit. mp 54-55° C., Noyce and Jorgenson, J. Am. Chem. Soc., 1963, 85, 2420-2426). 1H NMR (250 MHz) δ 8.33-8.26 (d, 1 H), 8.05-7.97 (m, 3 H), 7.57-7.49 (m, 3 H), 7.30 (m, 1 H), 6.61-6.57 (d, 2 H), 3.92 (s, 6 H); 13C NMR (62.7 MHz) 192.3, 160.6, 139.2, 136.0, 132.4, 131.7, 128.6, 125.1, 113.1, 105.8, 103.9, 56.0 ppm.

1. customa solid precipitated
2. customThe precipitate was recrystallized from methanol
3. customto afford 350 mg (87.1%) of a white, flaky solid