Sodium Hydroxide → N'-Hydroxy-2H-1,3-Benzodioxole-5-Carboximidamide
Reaktionsgleichung
O1[C:5]2[CH:6]=[CH:7][C:8]([C:10]#[N:11])=[CH:9][C:4]=2[O:3][CH2:2]1.Cl.[NH2:13][OH:14].[OH-:15].[Na+]>CCO>[OH:14][NH:13][C:10]([C:8]1[CH:7]=[CH:6][C:5]2[O:15][CH2:2][O:3][C:4]=2[CH:9]=1)=[NH:11]Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
To a solution of Benzo[1,3]dioxole-5-carbonitrile (5.0 g, 33.9 mmol) in EtOH (100 mL) was added hydroxylamine hydrochloride (4.68 g, 67.90 mmol) and NaOH (2.71 g, 67.9 mmol). The resulting reaction mixture was refluxed for 12 h. After the completion of the reaction (TLC monitoring), the mixture was concentrated, added EtOH and filtered. The filtrate was evaporated under reduced pressure and used as such for the next step (crude yield 4.8 g, 78.68%).
Aufarbeitung
- customThe resulting reaction mixture
- temperaturewas refluxed for 12 h
- customAfter the completion of the reaction (TLC monitoring)
- concentrationthe mixture was concentrated
- additionadded EtOH
- filtrationfiltered
- customThe filtrate was evaporated under reduced pressure
Quellen und Nachweise
- ORD-Eintrag
- ord-9b061b4b990849b49c3f77d2212db2d9
- Quelldatensatz
- uspto-grants-2012_01
- Patentnummer
- US08088791B2
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