Hydroxyamine hydrochloride → 3-Fluoro-2-trifluoromethyl-pyridine-4-carbaldehyde oxime

HRID 1527468Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1527468
[F:1][C:2]1[C:3]([C:10]([F:13])([F:12])[F:11])=[N:4][CH:5]=[CH:6][C:7]=1[CH:8]=O.Cl.[NH2:15][OH:16].C([O-])(=O)C.[NH4+]>CO.O>[F:1][C:2]1[C:3]([C:10]([F:13])([F:12])[F:11])=[N:4][CH:5]=[CH:6][C:7]=1[CH:8]=[N:15][OH:16]

Komponenten

6

Edukt 3

HCID 443297Hydroxyamine hydrochlorideHCID 517165Ammonium AcetateHCID 866738643-Fluoro-2-(trifluoromethyl)pyridine-4-carbaldehyde

Produkt 1

HCID 1363523253-Fluoro-2-trifluoromethyl-pyridine-4-carbaldehyde oxime

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

To a solution of 3-fluoro-2-trifluoromethyl-pyridine-4-carbaldehyde (0.495 g, 2.05 mmol) in MeOH (17.6 mL) and water (2.9 mL) were added hydroxylamine hydrochloride (0.214 g, 3.08 mmol) and ammonium acetate (0.474 g, 6.15 mmol), and the resulting mixture was stirred at RT overnight. Volatile were removed in vacuo, and the residue was suspended in CH2Cl2/MeOH 9:1. The precipitate was filtered off, washed with CH2Cl2 and dried to afford the title compound as a white solid. MS (LC/MS): 209.0 [M+H]+; tR (HPLC conditions c): 4.28 min.

Aufarbeitung

  1. customVolatile were removed in vacuo
  2. filtrationThe precipitate was filtered off
  3. washwashed with CH2Cl2
  4. customdried

Quellen und Nachweise

ORD-Eintrag
ord-423f296eef0f41c09ce34e77d16bcefb
Quelldatensatz
uspto-grants-2015_07
Patentnummer
US09085555B2

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