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Chloride → (R)-1-(3-(9H-tribenz[b,d,f]azepin-9-yl)propyl)-3-piperidine carboxylic acid ethyl ester hydrochloride

HRID 1290660
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1290660
[Cl-:1].[C:2]([CH:5]([CH:7]([C:9](O)=O)O)O)(O)=O.[NH:12]1[CH2:17][CH2:16][CH2:15][C@@H:14]([C:18]([O:20][CH2:21][CH3:22])=[O:19])[CH2:13]1.C(=O)([O-])[O-].[K+].[K+].[I-].[K+].[CH3:31][C:32](=O)[CH2:33][CH3:34]>ClCCl>[ClH:1].[CH2:21]([O:20][C:18]([C@@H:14]1[CH2:15][CH2:16][CH2:17][N:12]([CH2:18][CH2:14][CH2:13][N:12]2[C:33]3[CH:34]=[CH:2][CH:5]=[CH:7][C:32]=3[C:31]3[CH:15]=[CH:16][CH:17]=[CH:9][C:7]=3[C:5]3[CH:31]=[CH:32][CH:33]=[CH:34][C:2]2=3)[CH2:13]1)=[O:19])[CH3:22]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 5

HCID 312ChlorideHCID 4875Potassium IodideHCID 6569Methyl Ethyl KetoneHCID 11430Potassium CarbonateHCID 2733695(R)-(-)-Ethyl Nipecotate Tartrate

Produkt 1

HCID 70197521(R)-1-(3-(9H-tribenz[b,d,f]azepin-9-yl)propyl)-3-piperidine carboxylic acid ethyl ester hydrochloride
Ausbeute 41 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A mixture of the above chloride (0.21 g, 0.66 mmol), ethyl (R)-3-piperidinecarboxylate tartrate (0.30 g, 1.0 mmol), potassium carbonate (0.18 g, 2.0 mmol), potassium iodide (0.10 g, 0.60 mmol) and 2-butanone (10 ml) was heated at reflux temperature for 40 hours. After cooling to room temperature, dichloromethane (50 ml) was added and the mixture was filtered. The filtrate was washed with 1N hydrochloric acid (20 ml), water (20 ml) and saturated sodium hydrogencarbonate solution (20 ml), dried over sodium sulfate and evaporated in vacuo. The remainder was dissolved in diethyl ether (20 ml) and a 2.6M solution of hydrogen chloride in diethyl ether (0.5 ml) was added. The formed precipitate was collected by filtration, washed with ether and dried, affording 0.13 g (41%) of (R)-1-(3-(9H-tribenz[b,d,f]azepin-9-yl)propyl)-3-piperidine carboxylic acid ethyl ester hydrochloride as a solid.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureat reflux temperature for 40 hours
  3. filtrationthe mixture was filtered
  4. washThe filtrate was washed with 1N hydrochloric acid (20 ml), water (20 ml) and saturated sodium hydrogencarbonate solution (20 ml)
  5. dry with materialdried over sodium sulfate
  6. customevaporated in vacuo
  7. dissolutionThe remainder was dissolved in diethyl ether (20 ml)
  8. additiona 2.6M solution of hydrogen chloride in diethyl ether (0.5 ml) was added
  9. filtrationThe formed precipitate was collected by filtration
  10. washwashed with ether
  11. customdried

Quellen und Nachweise

ORD-Eintrag
ord-32652ec9efcc475c9fd1bb390b07416c
Quelldatensatz
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05753643

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