Hydrochloric Acid → HCID 23000985, Verbindung

HRID 397742Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 397742
[CH2:1]([N:7]1[CH2:12][CH2:11][CH:10]([C:13]2[CH:18]=[CH:17][CH:16]=[C:15]([NH:19]C(=O)C(O)(C)C)[CH:14]=2)[CH2:9][CH2:8]1)[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6].Cl>O1CCOCC1.O>[NH2:19][C:15]1[CH:14]=[C:13]([CH:10]2[CH2:11][CH2:12][N:7]([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH3:6])[CH2:8][CH2:9]2)[CH:18]=[CH:17][CH:16]=1

Komponenten

5

Edukt 2

HCID 313Hydrochloric AcidHCID 23001068HCID 23001068, Verbindung

Produkt 1

HCID 23000985HCID 23000985, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

A solution of N-hexyl-4-(3-(2-hydroxy-2-methylpropanoylamino)phenyl)piperidine (Example 158) in 1,4-dioxan:5N aqueous hydrochloric acid solution (1:1, 10 ml) was heated under reflux overnight. The reaction mixture was cooled, diluted with water (10 ml) and extracted with diethyl ether (3×10 ml). The pH of the aqueous layer was adjusted to 8-9 using 5N aqueous sodium hydroxide, and extracted with dichloromethane (5×10 ml). The combined extracts were washed with brine (10 ml), dried (Na2SO4) and concentrated in vacuo to give the title compound as an oil which was not purified further (178 mg, 61% over two steps).

Aufarbeitung

  1. temperatureunder reflux overnight
  2. temperatureThe reaction mixture was cooled
  3. extractionextracted with diethyl ether (3×10 ml)
  4. extractionextracted with dichloromethane (5×10 ml)
  5. washThe combined extracts were washed with brine (10 ml)
  6. dry with materialdried (Na2SO4)
  7. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-5cba0c1961d44f6790a509783b3bd4b5
Quelldatensatz
uspto-grants-2003_08
Patentnummer
US06610711B2

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