Acetic Acid → HCID 12370788, Verbindung

HRID 660324Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 660324
C([O:3][C:4](=[O:17])[CH:5]([C:7]1[CH:12]=[CH:11][C:10]([N+:13]([O-:15])=[O:14])=[C:9]([OH:16])[CH:8]=1)[CH3:6])C.[OH-].[Na+].C(O)(=O)C>CCO.O>[OH:16][C:9]1[CH:8]=[C:7]([CH:5]([CH3:6])[C:4]([OH:17])=[O:3])[CH:12]=[CH:11][C:10]=1[N+:13]([O-:15])=[O:14]

Komponenten

6

Edukt 3

HCID 176Acetic AcidHCID 14798Sodium HydroxideHCID 57742139HCID 57742139, Verbindung

Produkt 1

HCID 12370788HCID 12370788, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
45 °C

Versuchsvorschrift

To a stirred solution of 2-(3-Hydroxy-4-nitro-phenyl)-propionic acid ethyl ester (1.48 g) in 90% aq. EtOH was added NaOH (1.24 g) at room temperature. After stirred for 14 h at 45° C., the reaction mixture was cooled to room temperature, diluted with water. The resulting aqueous layer was acidified with acetic acid and then extracted with dichloromethane. The combined organic layer was dried over magnesium sulfate, filtered and concentrated in vacuo. (1.30 mg, 99.5%, yellow solid)

Aufarbeitung

  1. temperaturethe reaction mixture was cooled to room temperature
  2. extractionextracted with dichloromethane
  3. dry with materialThe combined organic layer was dried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-07085aa91fc847f0ba325171bd20f18a
Quelldatensatz
uspto-grants-2011_12
Patentnummer
US08084484B2

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