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Phenyl isocyanate → 4-[N-methyl-N-(2-phenylethyl)amino]-1-anilinocarbonylpiperidine

HRID 369182
ノート
印刷プレビュー

反応式

HRID 369182 の反応式
[C:1]1([N:7]=[C:8]=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:10][N:11]([CH:20]1[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]1)[CH2:12][CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1>C(Cl)(Cl)Cl>[CH3:10][N:11]([CH:20]1[CH2:21][CH2:22][N:23]([C:8]([NH:7][C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)=[O:9])[CH2:24][CH2:25]1)[CH2:12][CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=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 7672Phenyl isocyanateHCID 10856966Methyl-phenethyl-piperidin-4-YL-amine

生成物 1

HCID 232850024-[N-methyl-N-(2-phenylethyl)amino]-1-anilinocarbonylpiperidine

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

1.0 ml of phenyl isocyanate was added to a solution of 1.0 g of 4-[N-methyl-N-(2-phenylethyl)-amino]piperidine in 15 ml of chloroform. The mixture was stirred at room temperature for 2 hours. The reaction mixture was concentrated under reduced pressure. To the residue was added diethyl ether for crystallization. The resulting crystals were collected by filtration and recrystallized from ethyl acetate to obtain 0.7 g of 4-[N-methyl-N-(2-phenylethyl)amino]-1-anilinocarbonylpiperidine as colorless prism-like crystals.

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. additionTo the residue was added diethyl ether
  3. customfor crystallization
  4. filtrationThe resulting crystals were collected by filtration
  5. customrecrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-c4a9699bf6da44628938df8bc70dab54
出典データセット
uspto-grants-2000_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06136826

反応ノート

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