HRID372481

反应详情

EQUATION

反应方程式

HRID 372481 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
45 °C

PROCEDURE

实验过程

Trans ethyl 3-bromocinnamate (8.4 g), ethylamine (6.7 g), methanol (18 ml) and 4A molecular sieves (1 g) were combined and heated at reflux for 1/2 hour. The mixture was cooled to about 45° C and sodium methylate (0.6 g) added. The mixture was then heated at reflux 11/2 hour and then cooled. It was acidified with concentrated hydrochloric acid (12 ml). The sieves were removed by filtration. Ice water was added to the filtrate to precipitate trans 3-bromo-N-ethylcinnamamide, m.p. 89°-90° C (after recrystallization from ethanol/water).

WORKUP

后处理

  1. temperatureheated
  2. temperatureat reflux for 1/2 hour
  3. temperatureThe mixture was then heated
  4. temperatureat reflux 11/2 hour
  5. temperaturecooled
  6. customThe sieves were removed by filtration
  7. additionIce water was added to the filtrate
  8. customto precipitate
  9. customtrans 3-bromo-N-ethylcinnamamide, m.p. 89°-90° C (after recrystallization from ethanol/water)