1-(2,3-Xylyl)piperazine → HCID 13064841、化合物

HRID 1462530ノート

反応式

HRID 1462530 の反応式
[O:1]=[C:2]([C:6]1[CH:7]=[C:8]2[C:13](=[CH:14][CH:15]=1)[NH:12][C:11](=[O:16])[CH2:10][CH2:9]2)[CH2:3][CH2:4][Cl:5].[CH3:17][C:18]1[C:23]([CH3:24])=[CH:22][CH:21]=[CH:20][C:19]=1[N:25]1[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]1>C1(C)C(C)=CC=CC=1>[ClH:5].[O:1]=[C:2]([C:6]1[CH:7]=[C:8]2[C:13](=[CH:14][CH:15]=1)[NH:12][C:11](=[O:16])[CH2:10][CH2:9]2)[CH2:3][CH2:4][N:28]1[CH2:29][CH2:30][N:25]([C:19]2[CH:20]=[CH:21][CH:22]=[C:23]([CH3:24])[C:18]=2[CH3:17])[CH2:26][CH2:27]1

参加物

4

反応物 2

HCID 705411-(2,3-Xylyl)piperazineHCID 12833509HCID 12833509、化合物

生成物 1

HCID 13064841HCID 13064841、化合物

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

実験手順

2.4 Grams of 6-(1-oxo-3-chloropropyl)-3,4-dihydrocarbostyril and 4.5 g of 4-(2,3-dimethylphenyl)-piperazine were mixed with 80 ml of xylene and the mixture was refluxed by heating for 24 hours. Then the reaction mixture was concentrated under a reduced pressure to dryness. Thus obtained solid matter was dissolved in 100 ml of chloroform, the chloroform layer was washed with 5%-sodium hydrogencarbonate aqueous solution twice and washed with water twice then dried with anhydrous sodium sulfate, and chloroform was removed by distillation to obtain the residue. To the residue thus obtained was added ether-hexane and the insoluble matters were collected by filtration and recrystallized from concentrated hydrochloric acid-ethanol-water to obtain 2.6 g of 6-{1-oxo-3-[4-(2,3-dimethylphenyl)-1-piperazinyl]propyl}-3,4-dihydrocarbostyril monohydrochloride in colorless needle-like crystals.

後処理

  1. temperaturethe mixture was refluxed
  2. temperatureby heating for 24 hours
  3. concentrationThen the reaction mixture was concentrated under a reduced pressure to dryness
  4. dissolutionThus obtained solid matter was dissolved in 100 ml of chloroform
  5. washthe chloroform layer was washed with 5%-sodium hydrogencarbonate aqueous solution twice
  6. washwashed with water twice
  7. dry with materialdried with anhydrous sodium sulfate, and chloroform
  8. customwas removed by distillation
  9. customto obtain the residue
  10. customTo the residue thus obtained
  11. filtrationthe insoluble matters were collected by filtration
  12. customrecrystallized from concentrated hydrochloric acid-ethanol-water

出典と根拠

ORDレコード
ord-7fcc5152f5bf4b7c87eba27b68cfda35
出典データセット
uspto-grants-1984_07
特許番号
US04460593

反応ノート

読み込み中…