Lithium Hydroxide → 2,3-Dihydro-8-methoxy-1,4-benzodioxin-6-carboxylic acid

HRID 323401Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 323401
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:10]=[C:11]2[O:16][CH2:15][CH2:14][O:13][C:12]=12)[C:6]([O:8]C)=[O:7].[OH-].[Li+]>O1CCCC1>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:10]=[C:11]2[O:16][CH2:15][CH2:14][O:13][C:12]=12)[C:6]([OH:8])=[O:7]

Komponenten

4

Edukt 2

HCID 3939Lithium HydroxideHCID 18464946Methyl 8-Methoxy-2,3-dihydrobenzo[b][1,4]dioxine-6-carboxylate

Produkt 1

HCID 49623162,3-Dihydro-8-methoxy-1,4-benzodioxin-6-carboxylic acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

Combine methyl 3-methoxy-4,5-ethylenedioxybenzoate (0.46 g, 2.0 mmol) and tetrahydrofuran (15 mL). Add a 1 M aqueous solution of lithium hydroxide (2.5 mL, 2.5 mmol). Heat to reflux. After 15 hours, cool the reaction, concentrate in vacuo to remove most of the tetrahydrofuran. Cool in a ice bath and acidify with a 1 M aqueous hydrochloric acid solution to give a solid. Collect the solid by filtration and dry to give the title compound.

Aufarbeitung

  1. temperatureHeat to reflux
  2. temperaturecool
  3. customthe reaction
  4. concentrationconcentrate in vacuo
  5. customto remove most of the tetrahydrofuran
  6. temperatureCool in a ice bath
  7. customto give a solid
  8. customCollect the solid
  9. filtrationby filtration
  10. customdry

Quellen und Nachweise

ORD-Eintrag
ord-c575280252474660a52bde61ea2b6db1
Quelldatensatz
uspto-grants-2001_04
Patentnummer
US06211199B1

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