Hydroxyamine hydrochloride → N-hydroxy-1-[3-(methoxymethyl)phenyl]-1-(1-methyl-1H-tetrazol-5-yl)methanimine
Reaktionsgleichung
[CH3:1][O:2][CH2:3][C:4]1[CH:5]=[C:6]([C:10]([C:12]2[N:16]([CH3:17])[N:15]=[N:14][N:13]=2)=O)[CH:7]=[CH:8][CH:9]=1.Cl.[NH2:19][OH:20]>N1C=CC=CC=1>[OH:20][N:19]=[C:10]([C:6]1[CH:7]=[CH:8][CH:9]=[C:4]([CH2:3][O:2][CH3:1])[CH:5]=1)[C:12]1[N:16]([CH3:17])[N:15]=[N:14][N:13]=1Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 70 °C
Versuchsvorschrift
To a stirred solution of [3-(methoxymethyl)phenyl](1-methyl-1H-tetrazol-5-yl)methanone (7.17 g, 31 mmol) in dry pyridine (50 mL) was added hydroxylamine hydrochloride (5.36 g, 77 mmol). The reaction mixture was stirred at 70° C. for 4 h, then concentrated in vacuo and diluted with ethyl acetate (200 mL) and water (100 mL). The organic layer was separated, washed with water (100 mL) and dried (MgSO4). Evaporation of the solvent in vacuo afforded N-hydroxy-1-[3-(methoxymethyl)phenyl]-1-(1-methyl-1H-tetrazol-5-yl)methanimine as a yellow oil [8.43 g, yield 99.5%; HPLC/MS:m/z=248 (M+H); log P(HCOOH)=1.54].
Aufarbeitung
- concentrationconcentrated in vacuo
- additiondiluted with ethyl acetate (200 mL) and water (100 mL)
- customThe organic layer was separated
- washwashed with water (100 mL)
- dry with materialdried (MgSO4)
- customEvaporation of the solvent in vacuo
Quellen und Nachweise
- ORD-Eintrag
- ord-07d4aa6ec66b4381acd39db0f638caf0
- Quelldatensatz
- uspto-grants-2013_07
- Patentnummer
- US08492388B2
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