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Water → HCID 53873583, Verbindung

HRID 263470
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 263470
[OH:1][C:2]1[CH:12]=[CH:11][C:5]([CH:6]=[CH:7][C:8]([OH:10])=[O:9])=[CH:4][C:3]=1[N+:13]([O-:15])=[O:14].O.[C:17](OCC)(=[O:19])[CH3:18]>C(OC(=O)C)(=O)C.S(=O)(=O)(O)O>[C:17]([O:1][C:2]1[CH:12]=[CH:11][C:5]([CH:6]=[CH:7][C:8]([OH:10])=[O:9])=[CH:4][C:3]=1[N+:13]([O-:15])=[O:14])(=[O:19])[CH3:18]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 3

HCID 962WaterHCID 8857Ethyl AcetateHCID 534017683-(4-Hydroxy-3-nitrophenyl)prop-2-enoic acid

Produkt 1

HCID 53873583HCID 53873583, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 1118Sulfuric AcidKatalysatorHCID 7918Acetic Anhydride
Lösungsmittel

Versuchsvorschrift

10 g of 4-hydroxy-3-nitrocinnamic acid (prepared as described in Preparation 1) were dissolved in 30 ml of acetic anhydride. One drop of sulfuric acid was added to the solution, which was then stirred for 2 hours at room temperature. 50 ml of water were added the solution, and it was then stirred for a further 2 hours. At the end of this time, ethyl acetate was added, and the mixture was washed with water and with a saturated aqueous solution of sodium chloride, in that order, and then dried over anhydrous sodium sulfate. The solvent was removed by distillation under reduced pressure, and the residue was mixed with toluene; the remaining acetic acid was removed by azeotropic distillation to obtain 10.2 g of the title compound as crystals.

Aufarbeitung

  1. stirringwas then stirred for a further 2 hours
  2. washthe mixture was washed with water and with a saturated aqueous solution of sodium chloride, in that order
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvent was removed by distillation under reduced pressure
  5. additionthe residue was mixed with toluene
  6. customthe remaining acetic acid was removed by azeotropic distillation

Quellen und Nachweise

ORD-Eintrag
ord-98b3f75389d14d12a14eb31b8910e4ca
Quelldatensatz
uspto-grants-1997_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05643925

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