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Phenylhydrazine → 1-[beta-(2-Methyl-3-indolyl)propionyl]-4-phenylpiperazine

HRID 1580625
ノート
印刷プレビュー

反応式

HRID 1580625 の反応式
[C:1]1([NH:7]N)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:9]([CH2:12][CH2:13][CH2:14][C:15]([N:17]1[CH2:22][CH2:21][N:20]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[CH2:19][CH2:18]1)=[O:16])(=O)[CH3:10]>C(O)(=O)C>[CH3:10][C:9]1[NH:7][C:1]2[C:6]([C:12]=1[CH2:13][CH2:14][C:15]([N:17]1[CH2:22][CH2:21][N:20]([C:23]3[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=3)[CH2:19][CH2:18]1)=[O:16])=[CH:5][CH:4]=[CH:3][CH:2]=2
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 7516PhenylhydrazineHCID 215633821-(gamma-Acetylbutyryl)-4-phenylpiperazine

生成物 1

HCID 215634081-[beta-(2-Methyl-3-indolyl)propionyl]-4-phenylpiperazine

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

To a solution of 10.8 g of phenylhydrazine in 100 ml of 30 % aqueous acetic acid was added 27.4 g of 1-(γ-acetylbutyryl)-4-phenylpiperazine and the resulting mixture was stirred for 30 minutes at room temperature. The precipitate was filtered, and washed with water. The precipitate was added to 180 ml of 5 % ethanolic hydrogen chloride, and the mixture was heated under reflux for 4 hours. The solvent was distilled off under reduced pressure to the residue, to which was added 100 ml of water. The resulting solid substance was recrystallized from ethanol to give 1-[β-(2-methyl-3-indolyl)propionyl]-4-phenylpiperazine, melting at 120°-121°C.

後処理

  1. filtrationThe precipitate was filtered
  2. washwashed with water
  3. additionThe precipitate was added to 180 ml of 5 % ethanolic hydrogen chloride
  4. temperaturethe mixture was heated
  5. temperatureunder reflux for 4 hours
  6. distillationThe solvent was distilled off under reduced pressure to the residue, to which
  7. additionwas added 100 ml of water
  8. customThe resulting solid substance was recrystallized from ethanol

出典と根拠

ORDレコード
ord-a3f3562bf4ed4ef38fee530db75cd8bb
出典データセット
uspto-grants-1976_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03933824

反応ノート

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