HRID1700339

反应详情

EQUATION

反应方程式

HRID 1700339 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

306 mg (1.32 mmol) of N-methyl-3-oxo-N-(3-phenyl-2-propene-1-yl)butyramide, 0.150 ml (1.32 mmol) of 3-chlorobenzaldehyde and 0.013 ml (0.132 mmol) of piperidine were heated under reflux overnight while water was removed. After washing with water, the organic layer was dried over anhydrous magnesium sulfate and then the solvent was evaporated under reduced pressure. The residue and 204 mg (1.32 mmol) of 2-cyanoethyl 3-aminocrotonate were heated at 85° C. under stirring in 6.6 ml of 2-propanol overnight. The reaction mixture was further heated at 120° C. under stirring under atmospheric pressure for 3 hours while 2-propanol was evaporated. The residue was purified by the high-performance liquid chromatography to obtain the title compound.

WORKUP

后处理

  1. customwas removed
  2. washAfter washing with water
  3. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  4. customthe solvent was evaporated under reduced pressure
  5. customwas evaporated
  6. customThe residue was purified by the high-performance liquid chromatography