HRID6393

反应详情

EQUATION

反应方程式

HRID 6393 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 28.11 g (200 mmol) of 3-chlorobenzaldehyde, 15.4 g of ammonium acetate and 32.5 mL of nitromethane in 230 mL of glacial acetic acid was heated at reflux temperature for 3 h and then poured onto ice. The resultant aqueous mixture was made basic by the addition of 45% aqueous potassium hydroxide. The precipitate was filtered and crystallized from ethyl acetate/hexane to give 5 g of the title compound. The filtrate was concentrated to afford an additional 13.5 g of product.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux temperature for 3 h
  3. additionpoured onto ice
  4. filtrationThe precipitate was filtered
  5. customcrystallized from ethyl acetate/hexane