Hydroxylamine → N-Hydroxy-2-methoxy-benzamidine

HRID 336222

Reaktionsgleichung

Reaktionsgleichung von HRID 336222
[NH2:1][OH:2].[CH3:3][O:4][C:5]1[CH:12]=[CH:11][CH:10]=[CH:9][C:6]=1[C:7]#[N:8]>CCO>[OH:2][N:1]=[C:7]([C:6]1[CH:9]=[CH:10][CH:11]=[CH:12][C:5]=1[O:4][CH3:3])[NH2:8]

Komponenten

4

Edukt 2

HCID 787HydroxylamineHCID 810862-Methoxybenzonitrile

Produkt 1

HCID 4652214N-Hydroxy-2-methoxy-benzamidineAusbeute 100,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

Hydroxylamine (Fluka 55458; 50% in water; 11.28 mL; 187.76 mmol; 5 eq.) was added to a solution of 2-methoxybenzonitrile (Alrich 231231; 4.59 mL; 37.55 mmol; 1 eq.) in EtOH (50 mL) and the resulting mixture was stirred at room temperature for 16 hours then at 55° C. for 24 hours. The solvent was then evaporated and the resulting colourless oil was further dried under high vacuum to give a white solid. The latter was triturated in n-hexane, filtered and dried to afford the title compound (6.29 g, quantitative) as a white solid.

Aufarbeitung

  1. waitat 55° C. for 24 hours
  2. customThe solvent was then evaporated
  3. customthe resulting colourless oil was further dried under high vacuum
  4. customto give a white solid
  5. customThe latter was triturated in n-hexane
  6. filtrationfiltered
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-3425c79c891840548d6595d622922bcf
Quelldatensatz
uspto-grants-2014_11
Patentnummer
US08889668B2

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