Potassium Carbonate → HCID 178437966, Verbindung

HRID 558258Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 558258
[ClH:1].[NH2:2][OH:3].C(=O)([O-])[O-].[K+].[K+].[Cl:10][C:11]1[CH:12]=[C:13]([CH:27]=[C:28](Cl)[CH:29]=1)[O:14][C:15]1[C:16]([CH2:25][CH3:26])=[N:17][N:18]([CH2:22][C:23]#[N:24])[C:19]=1[CH2:20][CH3:21]>CO.O>[Cl:1][C:28]1[CH:27]=[C:13]([CH:12]=[C:11]([Cl:10])[CH:29]=1)[O:14][C:15]1[C:16]([CH2:25][CH3:26])=[N:17][N:18]([CH2:22][C:23](=[NH:24])[NH:2][OH:3])[C:19]=1[CH2:20][CH3:21]

Komponenten

6

Edukt 3

HCID 11430Potassium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 9880293HCID 9880293, Verbindung

Produkt 1

HCID 178437966HCID 178437966, VerbindungAusbeute 99,3 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

Hydroxylamine hydrochloride (1.1 g, 15.8 mmol) and potassium carbonate (2.1 g, 15.2 mmol) were added to a suspension of the nitrile (1 g, 3.1 mmol) of Example 4 in a mixture of methanol (25 ml) and water (10 ml) which was then heated under reflux for 3 days. After cooling, the mixture was extracted with dichloromethane (2×250 ml) and the combined organic layers were washed with brine (100 ml), dried over magnesium sulphate, filtered and concentrated under reduced pressure to afford the product as a white solid (1.1 g), m.p. 128-130° C.

Aufarbeitung

  1. temperaturewas then heated
  2. temperatureunder reflux for 3 days
  3. temperatureAfter cooling
  4. extractionthe mixture was extracted with dichloromethane (2×250 ml)
  5. washthe combined organic layers were washed with brine (100 ml)
  6. dry with materialdried over magnesium sulphate
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-cb98301426464ca69ef4e235acd76617
Quelldatensatz
uspto-grants-2011_11
Patentnummer
US08063044B2

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