Sulfuric Acid → HCID 19825785, Verbindung

HRID 2249210Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2249210
S(=O)(=O)(O)O.O[C:7]([CH:10]1[CH2:14][C:13]2[CH:15]=[C:16]([OH:21])[C:17]([O:19][CH3:20])=[CH:18][C:12]=2[O:11]1)([CH3:9])[CH3:8]>>[OH:21][C:16]1[C:17]([O:19][CH3:20])=[CH:18][C:12]2[O:11][C:10]([CH:7]([CH3:9])[CH3:8])=[CH:14][C:13]=2[CH:15]=1

Komponenten

3

Edukt 2

HCID 1118Sulfuric AcidHCID 19825784HCID 19825784, Verbindung

Produkt 1

HCID 19825785HCID 19825785, VerbindungAusbeute 43,5 %

Versuchsvorschrift

To a solution of conc. sulfuric acid (1 ml) was added 2,3-dihydro-2-(1-hydroxy-1-methylethyl)-6-methoxy-5-benzofuranol (50 mg) in several portions during a period of few minutes. The mixture was stirred for 10 minutes at ambient temperature and poured into ice water. The separated oil was extracted with methylene chloride. The organic layer was washed with water, dried, and concentrated in vacuo. The residue was purified by column chromatography on silica gel (n-hexane/methylene chloride =1/1) to yield 5-hydroxy-6-methoxy-2-(1-methylethyl)benzofuran (20 mg) as crystals.

Aufarbeitung

  1. extractionThe separated oil was extracted with methylene chloride
  2. washThe organic layer was washed with water
  3. customdried
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by column chromatography on silica gel (n-hexane/methylene chloride =1/1)

Quellen und Nachweise

ORD-Eintrag
ord-41ac6b771af64590ad03b6e1d14da17b
Quelldatensatz
uspto-grants-1991_08
Patentnummer
US05043354

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