Ammonium Hydroxide → 2,3-Difluoro-5-nitrophenol

HRID 1803151Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1803151
[OH-].[NH4+].C(=O)(OCC)[O:4][C:5]1[CH:10]=[C:9]([N+:11]([O-:13])=[O:12])[CH:8]=[C:7]([F:14])[C:6]=1[F:15]>CCOC(C)=O>[F:15][C:6]1[C:7]([F:14])=[CH:8][C:9]([N+:11]([O-:13])=[O:12])=[CH:10][C:5]=1[OH:4]

Komponenten

4

Edukt 2

HCID 14923Ammonium HydroxideHCID 66859069HCID 66859069, Verbindung

Produkt 1

HCID 221546562,3-Difluoro-5-nitrophenolAusbeute 85 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

Step M (3): Aqueous ammonium hydroxide (5 mL) was added to a solution of 2,3-difluoro-5-nitrophenyl ethyl carbonate (250 mg, 1.0 mol) in EtOAc (4 mL). The reaction mixture was quenched with 1 N HCl. The mixture was diluted with water and extracted with EtOAc. The organic layer was washed with brine, dried over sodium sulfate, filtered, and concentrated in vacuo to afford 2,3-difluoro-5-nitrophenol (150 mg, 85% yield).

Aufarbeitung

  1. customThe reaction mixture was quenched with 1 N HCl
  2. additionThe mixture was diluted with water
  3. extractionextracted with EtOAc
  4. washThe organic layer was washed with brine
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-960946d47f3c4bf8978c4a0ab66f48b5
Quelldatensatz
uspto-grants-2013_01
Patentnummer
US08349880B2

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