Hydroxyammonium hydrochloride → HCID 178513274, Verbindung

HRID 708977

Reaktionsgleichung

Reaktionsgleichung von HRID 708977
Cl[C:2]1[N:7]=[CH:6][C:5]([CH2:8][N+:9]2[C:14]([O-:15])=[C:13]([C:16]3[CH:21]=[CH:20][C:19]([C:22]#[N:23])=[CH:18][CH:17]=3)[C:12](=[O:24])[N:11]3[CH:25]=[CH:26][CH:27]=[CH:28][C:10]=23)=[CH:4][CH:3]=1.[ClH:29].[OH:30][NH3+:31].CC(C)([O-])C.[K+]>CS(C)=O.[Cl-].[Na+].O>[Cl:29][C:2]1[N:7]=[CH:6][C:5]([CH2:8][N+:9]2[C:14]([O-:15])=[C:13]([C:16]3[CH:21]=[CH:20][C:19]([C:22](=[NH:23])[NH:31][OH:30])=[CH:18][CH:17]=3)[C:12](=[O:24])[N:11]3[CH:25]=[CH:26][CH:27]=[CH:28][C:10]=23)=[CH:4][CH:3]=1

Komponenten

6

Edukt 3

HCID 22029257Hydroxyammonium hydrochlorideHCID 23665647Potassium tert-butoxideHCID 867092651-[(6-Chloro-3-pyridyl)methyl]-3-(4-cyanophenyl)-4-oxo-pyrido[1,2-a]pyrimidin-1-ium-2-olate2×

Produkt 1

HCID 178513274HCID 178513274, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 679Dimethyl SulfoxideLösungsmittelHCID 57417360Sodium chloride; waterLösungsmittel

Versuchsvorschrift

30 mg (0.08 mmol) of 1-[(6-chloro-3-pyridyl)methyl]-3-(4-cyanophenyl)-4-oxo-pyrido[1,2-a]pyrimidin-1-ium-2-olate (product of step 1) were dissolved in 2 ml DMSO. 13 mg (0.2 mmol) hydroxylammonium hydrochloride and 22 mg (0.2 mmol) potassium t-butoxide were added and the mixture was stirred at room temperature for 18 hours. The mixture was taken up with 10 ml of brine and extracted with ethyl acetate. The organic phases were dried with magnesium chloride and the solvent was removed under reduced pressure. The desired product was sufficiently pure without further purification (10 mg).

Aufarbeitung

  1. extractionextracted with ethyl acetate
  2. dry with materialThe organic phases were dried with magnesium chloride
  3. customthe solvent was removed under reduced pressure
  4. customThe desired product was sufficiently pure without further purification (10 mg)

Quellen und Nachweise

ORD-Eintrag
ord-19999677997c4cac96f8ae74ea9116a4
Quelldatensatz
uspto-grants-2015_11
Patentnummer
US09179680B2

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