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Aluminium lithium hydride → 3-Methyl-1-(phenylmethyl)-4-piperidinamine

HRID 1726449
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HRID 1726449 반응식
[CH2:1]([N:8]1[CH2:13][CH2:12][C:11](=[N:14]O)[CH:10]([CH3:16])[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[H-].[H-].[H-].[Li+].[Al+3]>C1COCC1>[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([NH2:14])[CH:10]([CH3:16])[CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
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참가 물질

4

반응물 2

HCID 21226445Aluminium lithium hydrideHCID 734153251-Benzyl-3-methyl-piperidin-4-one oxime

생성물 1

HCID 222788353-Methyl-1-(phenylmethyl)-4-piperidinamine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
50 °C

실험 절차

To a 25° C. solution of 1-benzyl-3-methyl-piperidin-4-one oxime in anhydrous THF (20 mL) was added LAH (1.0 M solution TBF), (15 mL, 15 mmol). After being stirred at 50° C. overnight, the resultant mixture was quenched with 20% KOH solution. The aqueous layer was extracted with CH2Cl2. The organic extracts were combined, washed with brine and dried over MgSO4. The solution was filtered and concentrated in vacuo to give the crude mixture ((±)-cis: (±)-trans=1:1) 1-benzyl-3-methyl-piperidin-4-ylamine (1). LC/MS m/z: 205 (M+H)+. This material was used without further purification.

후처리

  1. customthe resultant mixture was quenched with 20% KOH solution
  2. extractionThe aqueous layer was extracted with CH2Cl2
  3. washwashed with brine
  4. dry with materialdried over MgSO4
  5. filtrationThe solution was filtered
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-1f8717d33f1746e5bee2ad6c3a5df938
출처 데이터셋
uspto-grants-2009_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07491827B2

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