HRID1111130

反应详情

EQUATION

反应方程式

HRID 1111130 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture comprising 8.0 g of 4,5-dichloro-6-nitro-3(2H)pyridazinone, 29.75 g of 3-n-propoxy-4-methoxybenzylamine and 160 ml of ethanol, was refluxed under stirring for 15 hours. Ethanol was distilled off under reduced pressure, and water was added to the residue thereby obtained. The mixture was extracted with chloroform. The extract was washed with water and dried over sodium sulfate. Then, the solvent was distilled off to obtain an orange solid substance. This product was crystallized from a solvent mixture of methanol-water, to obtain 6.50 g of the above identified compound having a melting point of from 169° to 171° C. as orange crystals.

WORKUP

后处理

  1. temperaturewas refluxed
  2. distillationEthanol was distilled off under reduced pressure, and water
  3. additionwas added to the residue
  4. customthereby obtained
  5. extractionThe mixture was extracted with chloroform
  6. washThe extract was washed with water
  7. dry with materialdried over sodium sulfate
  8. distillationThen, the solvent was distilled off
  9. customto obtain an orange solid substance
  10. customThis product was crystallized from a solvent mixture of methanol-water
  11. customto obtain 6.50 g of the
  12. customof from 169° to 171° C.