HRID990904

反应详情

EQUATION

反应方程式

HRID 990904 的结构方程式

PROCEDURE

实验过程

(73) To a 0.33 M solution of 2,6-dichlorobenzaldehyde (1.75 g, 10 mmol) and acetone (290 mg, 5 mmol) in 30 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, 2H), 7.40-7.36 (d, 4H), 7.26-7.19 (d, 2H), 7.24-7.18 (m, 2H); 13C NMR (62.7 MHz) 189.1, 137.6, 135.4, 133.3, 132.5, 130.2, 129.1 ppm.

WORKUP

后处理

  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