反応 #3255

ord-b9d97a55e700483bba5a21fd55b4d6fd

反応条件

温度
60°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他obtained in reference example 2
  2. 2
    抽出extracted with chloroform
  3. 3
    乾燥The chloroform layer was dried over magnesium sulfate
  4. 4
    その他evaporated
  5. 5
    その他The residue was purified by silica gel column chromatography (eluent; chloroform:methanol=10:1(v/v)) and
  6. 6
    その他crystallized from ethyl acetate

実験手順

To a solution prepared with sodium (1.78 g, 77.4 mmol) and 2-dimethylaminoethanol (80 ml, 796 mmol) was added 6-chloro-9,10-methylenedioxy-7H-indeno[2,1-c]quinoline-7-on (8 g, 25.8 mmol) obtained in reference example 2, and the mixture was stirred with heat at 60° C. for 24 hours. The reaction mixture was poured into ice water and extracted with chloroform. The chloroform layer was dried over magnesium sulfate and evaporated. The residue was purified by silica gel column chromatography (eluent; chloroform:methanol=10:1(v/v)) and crystallized from ethyl acetate to give 6.37 g (yield: 68.1%) of title compound. The physicochemical properties thereof are shown in table 2.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05733918uspto-grants-1998_03