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Hydrogen chloride-ethyl acetate → HCID 68935247, Verbindung

HRID 1260926
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1260926
[Cl:1][C:2]1[CH:3]=[C:4]([C@H:9]2[C@H:14]([N:15]([CH3:24])[C:16]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)=[O:17])[CH2:13][CH2:12][N:11](C(OC(C)(C)C)=O)[CH2:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8].Cl.C(OCC)(=O)C>C(OCC)(=O)C>[Cl:1][C:2]1[CH:3]=[C:4]([C@H:9]2[C@H:14]([N:15]([CH3:24])[C:16](=[O:17])[C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[CH2:13][CH2:12][NH:11][CH2:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 86631305rel-1,1-Dimethylethyl (3R,4R)-4-(benzoylmethylamino)-3-(3,4-dichlorophenyl)-1-piperidinecarboxylate

Produkt 1

HCID 68935247HCID 68935247, VerbindungAusbeute 75,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To a solution of the compound (0.455 g) obtained in Example 13 in ethyl acetate (3 mL) was added 4N hydrogen chloride/ethyl acetate solution (3 mL), and the mixture was stirred at room temperature for 24 hr with heating. The reaction mixture was concentrated under reduced pressure, ethyl acetate was added to the residue, and the mixture was made basic with 2N aqueous sodium hydroxide solution. The organic layer was separated, washed with water, and the solvent was evaporated under reduced pressure to give the title compound (0.27 g, 75%) as a white powder.

Aufarbeitung

  1. temperaturewith heating
  2. concentrationThe reaction mixture was concentrated under reduced pressure, ethyl acetate
  3. additionwas added to the residue
  4. customThe organic layer was separated
  5. washwashed with water
  6. customthe solvent was evaporated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-0349a66488aa48f59f90d58cab307f0c
Quelldatensatz
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08470816B2

Notizen zur Reaktion

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