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Ethyl bromoacetate → (1,3-benzodioxol-5-yloxy)acetic acid

HRID 1767413
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1767413
[CH2:1]1[O:5][C:4]2[CH:6]=[C:7]([OH:10])[CH:8]=[CH:9][C:3]=2[O:2]1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:18][C:19]([O:21]CC)=[O:20]>CC(C)=O>[CH2:1]1[O:2][C:3]2[CH:9]=[CH:8][C:7]([O:10][CH2:18][C:19]([OH:21])=[O:20])=[CH:6][C:4]=2[O:5]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 7748Ethyl bromoacetateHCID 11430Potassium CarbonateHCID 68289Sesamol

Produkt 1

HCID 1531512(1,3-benzodioxol-5-yloxy)acetic acidAusbeute 11,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

The mixture of sesamol (270 mg, 2.0 mmol), potassium carbonate (910 mg, 6.6 mmol), ethyl bromoacetate (2.55 ml, 22.9 mmol) and acetone (25 ml) was refluxed for 21 h. After cooling, the mixture was filtered to remove potassium carbonate. The filtrate was concentrated under reduced pressure. To this residue, 20 ml dioxane and 14 ml 5% sodium hydroxide solution were added. After the uiixture was stirred at room temperature overnight, it was acidified with concentrated hydrochloric acid to pH 2, and then extracted three times with ethyl acetate (20 ml each). Organic phases were combined, washed with water and brine, dried over magnesium sulfate, filtered, and then evaporated in vacuo. The residue was recrystallized from chloroform and acetone to give 45 mg 3,4-methylenedioxyphenoxyacetic acid as white crystals, mp 149-151° C.

Aufarbeitung

  1. temperaturewas refluxed for 21 h
  2. temperatureAfter cooling
  3. filtrationthe mixture was filtered
  4. customto remove potassium carbonate
  5. concentrationThe filtrate was concentrated under reduced pressure
  6. additionTo this residue, 20 ml dioxane and 14 ml 5% sodium hydroxide solution were added
  7. extractionextracted three times with ethyl acetate (20 ml each)
  8. washwashed with water and brine
  9. dry with materialdried over magnesium sulfate
  10. filtrationfiltered
  11. customevaporated in vacuo
  12. customThe residue was recrystallized from chloroform and acetone

Quellen und Nachweise

ORD-Eintrag
ord-32ae8cf0e49b4c8786aa1717997b02a3
Quelldatensatz
uspto-grants-2007_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
USRE039707E1

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