Hydrochloric Acid → 2,9-dimethoxy-2,3-dihydro-7H-furo[3,2-g][1]benzopyran-7-one

HRID 1448509Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1448509
Cl.[OH:2][CH:3]1[O:18][C:6]2=[C:7]([O:16][CH3:17])[C:8]3[O:13][C:12](=[O:14])[CH:11]=[CH:10][C:9]=3[CH:15]=[C:5]2[CH2:4]1.[CH3:19]O>>[CH3:19][O:2][CH:3]1[O:18][C:6]2=[C:7]([O:16][CH3:17])[C:8]3[O:13][C:12](=[O:14])[CH:11]=[CH:10][C:9]=3[CH:15]=[C:5]2[CH2:4]1

Komponenten

4

Edukt 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 203802212-hydroxy-9-methoxy-2,3-dihydro-7H-furo[3,2-g][1]benzopyran-7-one

Produkt 1

HCID 203802262,9-dimethoxy-2,3-dihydro-7H-furo[3,2-g][1]benzopyran-7-one

Versuchsvorschrift

Dry methanol was saturated at 0° with gaseous hydrogen chloride. A sample of 0.576 g. (2.46 mmoles) of 2-hydroxy-9-methoxy-2,3-dihydro-7H-furo[3,2-g][1]benzopyran-7-one was dissolved in the resultant solution, and the dark reaction was allowed to proceed at room temperature for one hour. The solvent was evaporated and the residue was taken up in ethyl acetate/benzene. 1:4 and filtered through 50 g. silica, eluting with the same solvent system. Fractions containing the product, which is first eluted, were combined and evaporated to give pure 2,9-dimethoxy-2,3-dihydro-7H-furo[3,2-g][1]benzopyran-7-one as a white solid. Recrystallization from methanol afforded an analytical sample of this product, mp 131°-132°.

Aufarbeitung

  1. customthe dark reaction
  2. customThe solvent was evaporated
  3. filtration1:4 and filtered through 50 g
  4. washsilica, eluting with the same solvent system
  5. additionFractions containing the product, which
  6. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-e06d5de633754528ba421f4d97271f5d
Quelldatensatz
uspto-grants-1979_12
Patentnummer
US04180659

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