Potassium Carbonate → HCID 15219197, Verbindung

HRID 889279Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 889279
[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([F:15])[C:10]=1[N+:16]([O-])=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl[Sn]Cl.C([O-])([O-])=O.[K+].[K+]>CCO.Cl>[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([F:15])[C:10]=1[NH2:16])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

Komponenten

6

Edukt 3

HCID 11430Potassium CarbonateHCID 24479Stannous ChlorideHCID 578349821-(Benzyloxy)-3-fluoro-2-nitrobenzene

Produkt 1

HCID 15219197HCID 15219197, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 313Hydrochloric AcidLösungsmittelHCID 702EthanolLösungsmittel

Versuchsvorschrift

To a solution of 1-benzyloxy-3-fluoro-2-nitrobenzene (10.0 g, 40.5 mmol) in 100 mL of EtOH and 50 mL of 1N HCl is added SnCl2 (38.3 g, 202.5 mmol) and the solution is refluxed for 2 h. After cooling the mixture to RT, it is adjusted to PH>7 with solid K2CO3 and extracted with EtOAc. The organic layer is washed with water and brine, and dried over sodium sulfate. The solvent is removed under reduced pressure to give the product as a yellow liquid.

Aufarbeitung

  1. temperaturethe solution is refluxed for 2 h
  2. extractionextracted with EtOAc
  3. washThe organic layer is washed with water and brine
  4. dry with materialdried over sodium sulfate
  5. customThe solvent is removed under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-011329f9824a435a98b6edc478f88614
Quelldatensatz
uspto-grants-2012_08
Patentnummer
US08252820B2

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