Sodium Hydroxide → N-Hydroxybenzo[d][1,3]dioxole-5-carboximidamide

HRID 538607

Reaktionsgleichung

Reaktionsgleichung von HRID 538607
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

HCID 14798Sodium HydroxideHCID 78136Benzo-1,3-dioxole-5-carbonitrileHCID 443297Hydroxyamine hydrochloride

Produkt 1

HCID 178513224N-Hydroxybenzo[d][1,3]dioxole-5-carboximidamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

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

  1. customThe resulting reaction mixture
  2. temperaturewas refluxed for 12 h
  3. customAfter the completion of the reaction (TLC monitoring)
  4. concentrationthe mixture was concentrated
  5. additionadded EtOH
  6. filtrationfiltered
  7. customThe filtrate was evaporated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-ed4964eb1abe4136a714c129c4b0a833
Quelldatensatz
uspto-grants-2014_10
Patentnummer
US08865736B2

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