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1,1-Dichloroethane → 4-(Azetidin-1-yl)-1-benzylpiperidine dihydrochloride

HRID 492846
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HRID 492846 반응식
[ClH:1].[NH:2]1[CH2:5][CH2:4][CH2:3]1.[CH2:6]([N:13]1[CH2:18][CH2:17][C:16](=O)[CH2:15][CH2:14]1)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].[Cl:34]C(Cl)C.C(=O)([O-])[O-].[Na+].[Na+].Cl.C(OCC)(=O)C>O1CCCC1.[Cl-].[Na+].O.C(OCC)C.CCCCCC.C(OCC)(=O)C.O.C(O)(=O)C.C(N(CC)CC)C>[ClH:34].[ClH:1].[N:2]1([CH:16]2[CH2:15][CH2:14][N:13]([CH2:6][C:7]3[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=3)[CH2:18][CH2:17]2)[CH2:5][CH2:4][CH2:3]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

15

반응물 6

HCID 63651,1-DichloroethaneHCID 10340Sodium CarbonateHCID 192201-Benzyl-4-piperidoneHCID 5049666Sodium triacetoxyborohydrideHCID 12308726Azetidine hydrochlorideHCID 21866389Hydrogen chloride-ethyl acetate

생성물 1

HCID 23153398
4-(Azetidin-1-yl)-1-benzylpiperidine dihydrochloride

시약·촉매·용매 8

HCID 176Acetic Acid용매HCID 962Water용매HCID 3283Diethyl Ether용매HCID 8028Tetrahydrofuran용매HCID 8058Hexane용매HCID 8471Triethylamine용매HCID 8857Ethyl Acetate용매HCID 57417360Sodium chloride; water용매

실험 절차

Triethylamine (3.51 ml) was added to a suspension of azetidine hydrochloride (2.35 g) in tetrahydrofuran (60 ml). 1-Benzyl-4-piperidone (3.71 ml) and acetic acid (2.29 ml) were added thereto and the mixture was stirred in an ice bath. Sodium triacetoxyborohydride (6.36 g) and dichloroethane (60 ml) were further added, and the mixture was stirred for 3.3 hours at room temperature. After adding sodium carbonate to the reaction mixture until foaming ceased, water (50 ml), ethyl acetate (300 ml) and brine (50 ml) were added for partition. The aqueous layer was extracted with ethyl acetate (200 ml). The organic layers were combined and washed with saturated aqueous sodium hydrogencarbonate and dried over anhydrous sodium sulfate. The dried organic layer was concentrated under reduced pressure to provide a pale brown oil. This was dissolved in diethyl ether (20 ml)-hexane (20 ml) and a 4N hydrochloric acid-ethyl acetate solution (11 ml) was added. The precipitated solid was filtered and washed with hexane. This was subjected to aeration drying to provide a crude product of the title compound (6.55 g, quantitative) as a white solid.

후처리

  1. stirringthe mixture was stirred for 3.3 hours at room temperature
  2. customfor partition
  3. extractionThe aqueous layer was extracted with ethyl acetate (200 ml)
  4. washwashed with saturated aqueous sodium hydrogencarbonate
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationThe dried organic layer was concentrated under reduced pressure
  7. customto provide a pale brown oil
  8. filtrationThe precipitated solid was filtered
  9. washwashed with hexane
  10. customdrying

출처 및 근거

ORD 기록
ord-164d84365bc94ed6ad2562925029670b
출처 데이터셋
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07531532B2

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