Sodium Hydroxide → HCID 178491837, Verbindung

HRID 1963006Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1963006
[F:1][C:2]1[C:9]([O:10][CH3:11])=[CH:8][CH:7]=[C:6]([F:12])[C:3]=1[C:4]#[N:5].Cl.[NH2:14][OH:15].[OH-].[Na+]>CCO>[F:1][C:2]1[C:9]([O:10][CH3:11])=[CH:8][CH:7]=[C:6]([F:12])[C:3]=1[C:4]([NH:14][OH:15])=[NH:5]

Komponenten

5

Edukt 3

HCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 37918322,6-Difluoro-3-methoxybenzonitrile

Produkt 1

HCID 178491837HCID 178491837, VerbindungAusbeute 43,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

To a solution of 2,6-difluoro-3-methoxybenzonitrile (0.30 g, 1.70 mmol) in EtOH (10 ml) was added hydroxylamine hydrochloride (0.12 g, 1.70 mmol) and NaOH (0.071 g, 1.70 mmol). The resulting reaction mixture was refluxed for 15 h. After the completion of the reaction (TLC monitoring), the mixture was concentrated, added EtOH and filtered. The filtrate was evaporated in vacuo and the crude residue was purified over silica gel (60-120 M, 30% EtOAc-Hexane) to get the desired product (0.15 g, 42%) as a white solid.

Aufarbeitung

  1. customThe resulting reaction mixture
  2. temperaturewas refluxed for 15 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 in vacuo
  8. customthe crude residue was purified over silica gel (60-120 M, 30% EtOAc-Hexane)

Quellen und Nachweise

ORD-Eintrag
ord-4b8a3b32071b4f4ba96b0764b952141f
Quelldatensatz
uspto-grants-2013_04
Patentnummer
US08415383B2

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