反応 #2329046

ord-e632d8964a33431f84ca69436774fc38

反応条件

温度
130°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The reaction mixture is cooled to ambient temperature
  2. 2
    抽出The product is extracted with dichloromethane
  3. 3
    乾燥the organic layer is dried with sodium sulphate
  4. 4
    濃縮concentrated under reduced pressure
  5. 5
    その他The residue is recrystallized from N,N-dimethylformamide

実験手順

2.5 g benzoic acid (4-chloro-2H-phthalazin-1-ylidene)-hydrazide and 1 g triethylamine hydrochloride are suspended in 60 ml ethylene glycol and stirred at 130° C. for 3 h. The reaction mixture is cooled to ambient temperature and added to 600 ml water. The product is extracted with dichloromethane, the organic layer is dried with sodium sulphate and concentrated under reduced pressure. The residue is recrystallized from N,N-dimethylformamide to give the title compound.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07671050B2uspto-grants-2010_03