HRID649132

反应详情

EQUATION

反应方程式

HRID 649132 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2.51 g of 6-(3-bromophenyl)-3(2H)-pyridazinone, 5 ml of a 37% formalin and 2 drops of concentrated hydrochloric acid were dissolved in 50 ml of methanol, and then the solution was heated under reflux for about 7 hours. The mixture was then left to stand overnight, after which it was filtered and the filtrate was concentrated by evaporation under reduced pressure. The resulting residue was extracted with a 1:1 by volume mixture of ethyl acetate and acetone. After distilling the solvent from the extract, there were obtained 1.13 g (yield 40%) of the desired Compound No. 1 in the form of a white solid melting at 228°-229° C.

WORKUP

后处理

  1. temperaturethe solution was heated
  2. temperatureunder reflux for about 7 hours
  3. waitThe mixture was then left
  4. filtrationafter which it was filtered
  5. concentrationthe filtrate was concentrated by evaporation under reduced pressure
  6. extractionThe resulting residue was extracted with a 1:1 by volume mixture of ethyl acetate and acetone
  7. distillationAfter distilling the solvent from the extract