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Water → 4-(Azetidin-1-yl)piperidine dihydrochloride

HRID 492847
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HRID 492847 반응식
[ClH:1].Cl.[N:3]1([CH:7]2[CH2:12][CH2:11][N:10](CC3C=CC=CC=3)[CH2:9][CH2:8]2)[CH2:6][CH2:5][CH2:4]1.O>CC(O)C.[C].[Pd]>[ClH:1].[ClH:1].[N:3]1([CH:7]2[CH2:12][CH2:11][NH:10][CH2:9][CH2:8]2)[CH2:6][CH2:5][CH2:4]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 962WaterHCID 231533984-(Azetidin-1-yl)-1-benzylpiperidine dihydrochloride

생성물 1

HCID 231531084-(Azetidin-1-yl)piperidine dihydrochloride수율 185.1%

시약·촉매·용매 2

HCID 178418390HCID 178418390, 화합물촉매HCID 3776Isopropanol용매

실험 절차

After adding 10% palladium-carbon (600 mg) to a solution of the crude 4-(azetidin-1-yl)-1-benzylpiperidine dihydrochloride (6.55 g) in 2-propanol (50 ml)-water (50 ml), the mixture was stirred for 23 hours at room temperature under a hydrogen atmosphere. The catalyst was filtered and washed with 2-propanol, and then the filtrate was concentrated. Ethanol (10 ml)-hexane (50 ml) was added to the residue to produce suspended precipitate. It was then filtered and washed with 10 ml of ethanol. The filtered precipitate was subjected to aeration drying to provide the title compound (4.26 g) as white powder.

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후처리

  1. filtrationThe catalyst was filtered
  2. washwashed with 2-propanol
  3. concentrationthe filtrate was concentrated
  4. additionEthanol (10 ml)-hexane (50 ml) was added to the residue
  5. customto produce
  6. filtrationIt was then filtered
  7. washwashed with 10 ml of ethanol
  8. customdrying

출처 및 근거

ORD 기록
ord-b94a7eedcb6a491bb16c395c0a673a75
출처 데이터셋
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07531532B2

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