反应详情

(38) To a solution of benzaldehyde (295 mg, 2.77 mmol) and 2,6-dimethoxyacetophenone (500 mg, 2.77 mmol) in 4.1 ml of methanol was added 0.1 ml of 40% sodium hydroxide in water at 10° C. After stirring for 3 hour at room temperature, a solid appeared and was filtered. The precipitate was recrystallized from methanol to afford 371 mg (49.9%) of white flakes: mp 125.5-126.6° C. (lit. mp 123-124° C., Kuck and Grutzmacher, Org. Mass. Spect., 1978, 13, 90-102). 1H NMR (250 MHz) δ 7.55-7.51 (m, 2H), 7.39-7.30 (m, 5H), 7.00-6.94 (d, 1H), 6.64-6.61 (d, 2H), 3.79 (s, 6H); 13C NMR (62.7 MHz) 231.8, 176.1, 163.9, 153.4, 149.4, 149.0, 147.4, 147.3, 147.0, 122.6, 74.5 ppm.

1. filtrationwas filtered
2. customThe precipitate was recrystallized from methanol
3. customto afford 371 mg (49.9%) of white flakes