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

HRID 1588967노트

반응식

HRID 1588967 반응식
[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

참가 물질

7

반응물 4

HCID 962Water2회HCID 14798Sodium HydroxideHCID 109900971-Benzyl-4-phenyl-piperazine-2-carboxamideHCID 21226445Aluminium lithium hydride

생성물 1

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

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 21226129Dichloromethane methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7b5211e729524e96b1db4125f7043490
출처 데이터셋
uspto-grants-1993_06
특허 번호
US05223623

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