Water → C-(1-Benzyl-4-phenyl-piperazin-2-yl)-methylamine

HRID 1588967ノート

反応式

HRID 1588967 の反応式
[C:1]1([N:7]2[CH2:12][CH2:11][N:10]([CH2:13][C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[CH:9]([C:20]([NH2:22])=O)[CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCCC1.C(Cl)Cl.CO>[C:1]1([N:7]2[CH2:12][CH2:11][N:10]([CH2:13][C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[CH:9]([CH2:20][NH2:22])[CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

7

反応物 4

HCID 962Water2 回HCID 14798Sodium HydroxideHCID 109900971-Benzyl-4-phenyl-piperazine-2-carboxamideHCID 21226445Aluminium lithium hydride

生成物 1

HCID 11044210C-(1-Benzyl-4-phenyl-piperazin-2-yl)-methylamine

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 21226129Dichloromethane methanol溶媒

実験手順

To 4-phenyl-1-(phenylmethyl)-2-piperazinecarboxamide (28.5 g, 96 mmol) dissolved in tetrahydrofuran (220 mL) add lithium aluminum hydride (9.0 g, 0.24 mol) portionwise. Stir and heat the reaction to reflux. Monitor the progress of the reaction by thin-layer chromatography. Upon completion, slowly add water (9 mL), 2N NaOH (9 ml), and H2O (27 mL). Suction filter the slurry through celite and wash the pad with ethyl acetate (500 mL). Remove the solvent in vacuo to give a brown oil. Flash chromatograph the oil on silica (400 g) with 19/1 CH2Cl2 /MeOH to give the title compound.

後処理

  1. temperatureheat
  2. customthe reaction
  3. temperatureto reflux
  4. customMonitor the progress of the reaction by thin-layer chromatography
  5. filtrationSuction filter the slurry through celite
  6. washwash the pad with ethyl acetate (500 mL)
  7. customRemove the solvent in vacuo
  8. customto give a brown oil

出典と根拠

ORDレコード
ord-7b5211e729524e96b1db4125f7043490
出典データセット
uspto-grants-1993_06
特許番号
US05223623

反応ノート

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