反应详情

(73) To a 0.33 M solution of 2,6-dichlorobenzaldehyde (1.75 g, 10 mmol) and acetone (290 mg, 5 mmol) in 30 ml of ethanol was added 5 ml of 40% potassium hydroxide at 10° C. After stirring for 18 hr at room temperature, a solid precipitated and was filtered. The precipitate was recrystallized from ethanol to afford 1.46 g (78.5%) of pale yellow, cotton-like flakes: mp 154.0-154.4° C. (lit. mp 145-146° C., Unterhalt, Arch. Pharm., 1978, 311, 262-267). 1H NMR (250 MHz) δ 7.85-7.79 (d, 2 H), 7.40-7.36 (d, 4 H), 7.26-7.19 (d, 2 H), 7.24-7.18 (m, 2 H); 13C NMR (62.7 MHz) 189.1, 137.6, 135.4, 133.3, 132.5, 130.2, 129.1 ppm.

1. customa solid precipitated
2. filtrationwas filtered
3. customThe precipitate was recrystallized from ethanol
4. customto afford 1.46 g (78.5%) of pale yellow, cotton-like flakes