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Hydrazine → 3-(4-(4-Fluorophenyl)piperidin-1-yl)propan-1-amine

HRID 1977805
ノート
印刷プレビュー

反応式

HRID 1977805 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][CH2:16]C3C=CC=C4C(NC(=O)C=34)=O)[CH2:10][CH2:9]2)=[CH:4][CH:3]=1.[NH2:28]N>CO>[F:1][C:2]1[CH:3]=[CH:4][C:5]([CH:8]2[CH2:9][CH2:10][N:11]([CH2:14][CH2:15][CH2:16][NH2:28])[CH2:12][CH2:13]2)=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 9321HydrazineHCID 227294733-[4-(4-Fluorophenyl)piperidin-1-yl]propylphthalimide

生成物 1

HCID 101985993-(4-(4-Fluorophenyl)piperidin-1-yl)propan-1-amine

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 3-[4-(4-fluorophenyl)piperidin-1-yl] propylphthalimide (4.5 g, 12.3 mmol) in methanol (200 mL) was added 4 ml of hydrazine and the mixture was stirred and refluxed for 8 h. It was cooled, and the white solid was filtered and washed with methanol (20 mL). Solvent was evaporated, and the residue was dried under vacuum for 4 h. Chloroform (50 mL) was added to this material, it was stirred for 1 h and filtered. The white solid was washed with more chloroform (20 mL), and the solvent was evaporated from the combined filtrates to leave the crude product as an oil. It was purified by column chromatography on silica gel using dichloromethane/methanol/2M ammonia in methanol (10/3/1) as the eluent.

後処理

  1. temperaturerefluxed for 8 h
  2. temperatureIt was cooled
  3. filtrationthe white solid was filtered
  4. washwashed with methanol (20 mL)
  5. customSolvent was evaporated
  6. customthe residue was dried under vacuum for 4 h
  7. additionChloroform (50 mL) was added to this material, it
  8. stirringwas stirred for 1 h
  9. filtrationfiltered
  10. washThe white solid was washed with more chloroform (20 mL)
  11. customthe solvent was evaporated from the combined filtrates

出典と根拠

ORDレコード
ord-4bb742027cc24fcba5585e6eac6e188a
出典データセット
uspto-grants-2001_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06235759B1

反応ノート

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