HRID1381484

反应详情

EQUATION

反应方程式

HRID 1381484 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A slurry composed of 1-(4-carboxyphenyl)-3-methyl-2-pyrazolin-5-one (21.8 gm, 0.10 mol), 4-dimethylaminobenzaldehyde (14.9 gm, 0.10 mol) and EtOH (250 ml) was heated at reflux for two hours. The reaction mixture was cooled to RT resulting in a crude orange product which was isolated by filtration. The product was then washed with ether and dried. The product was purified further by making a slurry of the solid in EtOH (700 ml) at refluxing temperature and filtering the slurry to recover the dye. The treatment was repeated. The mp of the product was above 310° C. The NMR and IR spectra were consistent with the structure assigned. The C,H, and N elemental analyses were in agreement with those calculated for the empirical formula.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for two hours
  3. customresulting in a crude orange product which
  4. customwas isolated by filtration
  5. washThe product was then washed with ether
  6. customdried
  7. customThe product was purified further
  8. temperatureat refluxing temperature
  9. filtrationfiltering the slurry
  10. customto recover the dye
  11. customwas above 310° C