Hydroxyamine hydrochloride → 5-Bromo-4-methyl-pyridine-2-carbaldehyde oxime

HRID 1027594Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1027594
[Br:1][C:2]1[C:3]([CH3:10])=[CH:4][C:5]([CH:8]=O)=[N:6][CH:7]=1.Cl.[NH2:12][OH:13].C([O-])(=O)C.[Na+]>CCO.O>[Br:1][C:2]1[C:3]([CH3:10])=[CH:4][C:5]([CH:8]=[N:12][OH:13])=[N:6][CH:7]=1

Komponenten

6

Edukt 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 594745005-Bromo-4-methylpicolinaldehyde

Produkt 1

HCID 1363413885-Bromo-4-methyl-pyridine-2-carbaldehyde oximeAusbeute 66 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

To a solution of the compound obtained in Step B (3.1 g) in EtOH (47.5 ml) and water (23 ml) were added hydroxylamine hydrochloride (1.4 g) and sodium acetate (1.9 g). The reaction was stirred for 15 min at room temperature. The white solid was filtered off and the solution concentrated in vacuo to afford the crude title product (2.2 g, white solid), which was used directly for the next step. LCMS (Method F) 2.09 min, M+H 564/566.

Aufarbeitung

  1. filtrationThe white solid was filtered off
  2. concentrationthe solution concentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-81b2912c0bab483b8928743b60cccea6
Quelldatensatz
uspto-grants-2014_05
Patentnummer
US08735362B2

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