HRID557416

反应详情

EQUATION

反应方程式

HRID 557416 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Methyl-4-oxo-4H-chromene-8-carbaldehyde (2 g, 10.62 mmol) and propyl acetoacetate (1.53 g, 10.62 mmol) are dissolved in 500 ml of dichloromethane and, after addition of glacial acetic acid (0.76 ml, 13.28 mmol) and piperidine (0.1 ml, 1.06 mmol), heated under reflux with a water trap for 18 h. After cooling, the reaction mixture is diluted with 50 ml of dichloromethane and washed with 20 ml of sodium chloride solution, the organic phase is dried over sodium sulfate, and the solvent is removed in vacuo. 3.3 g (99% of theory) of the title compound are obtained as an E/Z isomer mixture.

WORKUP

后处理

  1. temperatureheated
  2. temperatureunder reflux with a water trap for 18 h
  3. temperatureAfter cooling
  4. washwashed with 20 ml of sodium chloride solution
  5. dry with materialthe organic phase is dried over sodium sulfate
  6. customthe solvent is removed in vacuo