HRID441560
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureheated
- temperatureat reflux for 1/2 hour
- temperatureThe mixture was then heated
- temperatureat reflux 11/2 hour
- temperaturecooled
- customThe sieves were removed by filtration
- additionIce water was added to the filtrate
- customto precipitate
- customtrans 3-bromo-N-ethylcinnamamide, m.p. 89°-90° C. (after recrystallization from ethanol/water)