HRID557435

反应详情

EQUATION

反应方程式

HRID 557435 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

100 mg (0.53 mmol) of 2-methyl-4-oxo-4H-chromene-8-carbaldehyde are dissolved with 105 mg (0.53 mmol) of isopropyl 4,4,4-trifluoro-3-oxobutanoate, 43.6 mg (0.53 mmol) of 3-aminocrotononitrile and 46 μl (0.79 mmol) of acetic acid in 5 ml of 2-propanol and heated under reflux under argon for 4 h. The solvent is removed in vacuo, and the residue is purified by preparative HPLC. The main product obtained in this way is stirred under reflux in acetic acid overnight. The solution is concentrated and the residue is recrystallized from diethyl ether. 75 mg (33% of theory) of the title compound are obtained as a white solid.

WORKUP

后处理

  1. temperatureheated
  2. temperatureunder reflux under argon for 4 h
  3. customThe solvent is removed in vacuo
  4. customthe residue is purified by preparative HPLC
  5. customThe main product obtained in this way
  6. concentrationThe solution is concentrated
  7. customthe residue is recrystallized from diethyl ether