Hydroxylamine → HCID 178526331, Verbindung

HRID 574697

Reaktionsgleichung

Reaktionsgleichung von HRID 574697
[NH:1]1[C:5]2[CH:6]=[CH:7][C:8]([CH:10]=O)=[CH:9][C:4]=2[N:3]=[CH:2]1.[NH2:12][OH:13].O.O.O.C([O-])(=O)C.[Na+].C(OCC)(=O)C>CO>[NH:1]1[C:5]2[CH:6]=[CH:7][C:8]([CH:10]=[N:12][OH:13])=[CH:9][C:4]=2[N:3]=[CH:2]1

Komponenten

6

Versuchsvorschrift

1H-benzo[d]imidazole-5-carbaldehyde (0.57 mmol, 1 eq.) was dissolved in 5 mL methanol, hydroxylamine (0.68 mmol, 1.2 eq.) and sodium acetate trihydrate (0.68 mmol, 1.2 eq.) were added. The mixture was stirred for 1 hour at ambient temperature. 20 mL Ethyl acetate was added and the organic layer was washed with 20 mL of brine. The organic layer was dried over magnesium sulfate, filtrated and the solvent was removed under reduced pressure. The product was purified by means of flash-chromatography using silica gel and a ethyl acetate/MeOH-gradient.

Aufarbeitung

  1. washthe organic layer was washed with 20 mL of brine
  2. dry with materialThe organic layer was dried over magnesium sulfate
  3. filtrationfiltrated
  4. customthe solvent was removed under reduced pressure
  5. customThe product was purified by means of flash-chromatography

Quellen und Nachweise

ORD-Eintrag
ord-bde9e35a5f2449c097bc85ff4f41d369
Quelldatensatz
uspto-grants-2015_05
Patentnummer
US09034907B2

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