Hydrochloric Acid → 1-[2-(4-amino-1-piperidinyl)ethyl]-7-fluoro-2(1H)-quinoxalinone dihydrochloride

HRID 656943Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 656943
[F:1][C:2]1[CH:11]=[C:10]2[C:5]([N:6]=[CH:7][C:8](=[O:28])[N:9]2[CH2:12][CH2:13][N:14]2[CH2:19][CH2:18][CH:17]([NH:20]C(=O)OC(C)(C)C)[CH2:16][CH2:15]2)=[CH:4][CH:3]=1.[ClH:29]>CO.C(Cl)Cl.O1CCOCC1>[ClH:29].[ClH:29].[NH2:20][CH:17]1[CH2:16][CH2:15][N:14]([CH2:13][CH2:12][N:9]2[C:10]3[C:5](=[CH:4][CH:3]=[C:2]([F:1])[CH:11]=3)[N:6]=[CH:7][C:8]2=[O:28])[CH2:19][CH2:18]1

Komponenten

6

Edukt 2

HCID 313Hydrochloric AcidHCID 59397942tert-butyl{1-[2-(7-fluoro-2-oxoquinoxalin-1(2H)-yl)ethyl]piperidin-4-yl}carbamate

Produkt 1

HCID 688175421-[2-(4-amino-1-piperidinyl)ethyl]-7-fluoro-2(1H)-quinoxalinone dihydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 887MethanolLösungsmittelHCID 6344DichloromethaneLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

A solution of 1,1-dimethylethyl {1-[2-(7-fluoro-2-oxo-1(2H)-quinoxalinyl)ethyl]-4-piperidinyl}carbamate (4.0 g) in dry MeOH (15 ml) and dry DCM (30 ml) was treated with 4 M hydrogen chloride in 1,4-dioxane (30 ml) and stirred at rt for 3 h. It was evaporated to dryness and the insoluble product was heated in MeOH (50 ml), cooled, filtered, washed with cold MeOH, then ether, to give a solid (3.05 g).

Aufarbeitung

  1. customIt was evaporated to dryness
  2. temperaturethe insoluble product was heated in MeOH (50 ml)
  3. temperaturecooled
  4. filtrationfiltered
  5. washwashed with cold MeOH

Quellen und Nachweise

ORD-Eintrag
ord-bc5bdbbbba6f47a1814e09d0deb45f80
Quelldatensatz
uspto-grants-2011_12
Patentnummer
US08071592B2

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