反応 #2378381

ord-24be9d75f83247d985f17798863f616c

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度refluxed
  2. 2
    温度by heating for 5 hours
  3. 3
    workup.ADDITIONThen 3 g of activated carbon was added to the reaction mixture
  4. 4
    ろ過filtered with Celite
  5. 5
    濃縮the mother liquor was concentrated under a reduced pressure
  6. 6
    その他to obtain a residue
  7. 7
    その他The residue was purified by a silica-gel chromatography
  8. 8
    その他recrystallized from isopropanol

実験手順

2.87 Grams of 6-(3-piperazinylpropyl)-3,4-dihydrocarbostyril, 2.0 g of p-nitroaniline, 0.8 g of potassium carbonate and 0.2 g of copper power were mixed in 80 ml of 3-methoxybutanol and refluxed by heating for 5 hours. Then 3 g of activated carbon was added to the reaction mixture and filtered with Celite, then the mother liquor was concentrated under a reduced pressure to obtain a residue. The residue was purified by a silica-gel chromatography and recrystallized from isopropanol to obtain 0.55 g of 6-{3-[4-(4-nitrophenyl)-1-piperazinyl]propyl}-3,4-dihydrocarbostyril in yellow needle-like crystals, having the melting point of 189°-192° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04619932uspto-grants-1986_10