HRID1769141

反应详情

EQUATION

反应方程式

HRID 1769141 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Methyl hydrazine (8.05 g, 0.175 mol) was added to a mixture of 2-(4-isopropylbenzoyl)benzoic acid (40.2 g, 0.15 mol) in toluene (350 mL) and the mixture was heated to reflux for 3 hours with the removal of water with a Dean Stark trap. The reaction mixture was hot filtered through celite, the filtrate was concentrated to 125 mL and the filtrate was diluted with hexane (100 mL) and cooled. A solid was collected by filtration to afford 27.97 g (67%) of 2-methyl-4-(4-isopropylphenyl)-1-(2H)-phthalazinone, m.p. 107°-107.5° C.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. filtrationThe reaction mixture was hot filtered through celite
  3. concentrationthe filtrate was concentrated to 125 mL
  4. additionthe filtrate was diluted with hexane (100 mL)
  5. temperaturecooled
  6. filtrationA solid was collected by filtration