HRID441561

反应详情

EQUATION

反应方程式

HRID 441561 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of trans 3-bromocinnamoyl chloride (5 g) in dry benzene (100 ml) was added with stirring to an ethereal (200 ml) solution of methylamine (3 g). After the addition was complete, a slow stream of methylamine gas was bubbled through the reaction mixture at room temperature for 1 hour. Solvent and excess amine were removed under reduced pressure. The crude product was triturated with water, filtered, and recrystallized from ethanol-water to give trans 3-bromo-N-methylcinnamamide, m.p. 147°-147.5° C. NMR, IR, and elemental analysis were consistent with this structure.

WORKUP

后处理

  1. additionAfter the addition
  2. customa slow stream of methylamine gas was bubbled through the reaction mixture at room temperature for 1 hour
  3. customSolvent and excess amine were removed under reduced pressure
  4. customThe crude product was triturated with water
  5. filtrationfiltered
  6. customrecrystallized from ethanol-water