HRID2254511

反应详情

EQUATION

反应方程式

HRID 2254511 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

The camphor (50.2 g, 0.33 mol), dimethoxyethane (180 ml) and sodium hydride (32 g at 50% in oil, 0.33 mol) washed with dimethoxyethane, are placed in a round-bottom flask. The mixture is heated under nitrogen to 80° C. and the meta-nitrobenzaldehyde (45.3 g, 0.3 mol) dissolved in dimethoxyethane (100 ml) is added dropwise over half an hour. The mixture is left stirring at 80° C. for 1.5 hours. The reaction mixture is allowed to cool and it is poured cautiously in 2 litres of acidified and ice cold water. The brown precipitate obtained is filtered, washed with water and dried. After recrystallisation in diisopropyl ether in the presence of vegetable black, 20 g of meta-nitrobenzylidenecamphor are obtained.

WORKUP

后处理

  1. customare placed in a round-bottom flask
  2. additionis added dropwise over half an hour
  3. waitThe mixture is left
  4. temperatureto cool
  5. additionit is poured cautiously in 2 litres
  6. customThe brown precipitate obtained
  7. filtrationis filtered
  8. washwashed with water
  9. customdried
  10. customAfter recrystallisation in diisopropyl ether in the presence of vegetable black, 20 g of meta-nitrobenzylidenecamphor
  11. customare obtained