Dimethyl Sulfate → 4-(4-Methoxy-3-ethoxyphenyl)-3-buten-2-one

HRID 38666

Reaktionsgleichung

Reaktionsgleichung von HRID 38666
[C:1](=O)([O-])[O-].[Na+].[Na+].S(OC)(OC)(=O)=O.[OH:14][C:15]1[CH:20]=[CH:19][C:18]([CH:21]=[CH:22][C:23](=[O:25])[CH3:24])=[CH:17][C:16]=1[O:26][CH2:27][CH3:28]>CC(C)=O>[CH3:1][O:14][C:15]1[CH:20]=[CH:19][C:18]([CH:21]=[CH:22][C:23](=[O:25])[CH3:24])=[CH:17][C:16]=1[O:26][CH2:27][CH3:28]

Komponenten

5

Edukt 3

HCID 6497Dimethyl SulfateHCID 10340Sodium CarbonateHCID 692474294-(3-Ethoxy-4-hydroxyphenyl)but-3-en-2-one

Produkt 1

HCID 539602744-(4-Methoxy-3-ethoxyphenyl)-3-buten-2-oneAusbeute 65,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

Anhydrous sodium carbonate (3.98 g) and dimethyl sulfate (3.78 g, 30 mmol) were added to a solution of 4-(4-hydroxy-3-ethoxyphenyl)-3-buten-2-one (6.2 g, 30 mmol) in acetone (40 ml). The reaction mixture was stirred under refluxing for 8 hr. The precipitated yellow solid was filtered, washed with acetone, and then recrystallized from anhydrous ethanol to give 4.3 g of a yellow crystal, mp 95-96° C., yield 65.3%.

Aufarbeitung

  1. temperatureunder refluxing for 8 hr
  2. filtrationThe precipitated yellow solid was filtered
  3. washwashed with acetone
  4. customrecrystallized from anhydrous ethanol

Quellen und Nachweise

ORD-Eintrag
ord-78ec42e1d23b4d7b91bc52b5997e61ff
Quelldatensatz
uspto-grants-2013_09
Patentnummer
US08524744B2

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