StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

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

HRID 492846
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 492846
[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
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

15

Edukt 6

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

Produkt 1

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

Reagenzien, Katalysatoren, Lösungsmittel 8

HCID 176Acetic AcidLösungsmittelHCID 962WaterLösungsmittelHCID 3283Diethyl EtherLösungsmittelHCID 8028TetrahydrofuranLösungsmittelHCID 8058HexaneLösungsmittelHCID 8471TriethylamineLösungsmittelHCID 8857Ethyl AcetateLösungsmittelHCID 57417360Sodium chloride; waterLösungsmittel

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-164d84365bc94ed6ad2562925029670b
Quelldatensatz
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07531532B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion