Hydroxylamine HCl → N-hydroxy-1-(1-methyl-1H-tetrazol-5-yl)-1-phenylmethanimine

HRID 350956

Reaktionsgleichung

[CH3:1][N:2]1[C:6]([C:7]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=O)=[N:5][N:4]=[N:3]1.[Cl-].[OH:16][NH3+:17]>N1C=CC=CC=1>[CH3:1][N:2]1[C:6]([C:7]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[N:17][OH:16])=[N:5][N:4]=[N:3]1

Komponenten

Reaktionsbedingungen

Temperatur: 45 °C

Versuchsvorschrift

(1-methyltetrazol-5-yl)phenylmethanone (11.1 g, 59.1 mmol) and hydroxylammonium chloride (10.3 g, 148 mmol) were added to 100 ml of pyridine, followed by stirring at 45° C. for 24 hours. After the completion of the reaction, the reaction solution was concentrated under reduced pressure and water and ethyl acetate were added to the resulting residue, and then the reaction product was extracted. The organic layer was washed in turn with dilute hydrochloric acid, water and an aqueous sodium hydrogencarbonate, and the organic layer was dried over anhydrous magnesium sulfate. The solvent was distilled off from the organic layer to obtain (1-methyltetrazol-5-yl)phenylmethanoneoxime (12.0 g, yield: 100%) represented by the formua:

Aufarbeitung

customAfter the completion of the reaction
concentrationthe reaction solution was concentrated under reduced pressure and water and ethyl acetate
additionwere added to the resulting residue
extractionthe reaction product was extracted
washThe organic layer was washed in turn with dilute hydrochloric acid, water
dry with materialan aqueous sodium hydrogencarbonate, and the organic layer was dried over anhydrous magnesium sulfate
distillationThe solvent was distilled off from the organic layer

Quellen und Nachweise

ORD-Eintrag: ord-ed8ca4e8b684411eb7408c665a9f1654
Quelldatensatz: uspto-grants-2007_02
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US07183299B2

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