Sulfuric Acid → Methyl 9-hydroxy-9H-fluorene-9-carboxylate

HRID 33419

Reaktionsgleichung

Reaktionsgleichung von HRID 33419
[OH:1][C:2]1([C:15]([OH:17])=[O:16])[C:14]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=2[C:8]2[C:3]1=[CH:4][CH:5]=[CH:6][CH:7]=2.S(=O)(=O)(O)O.[C:23](=O)([O-])O.[Na+]>CO>[OH:1][C:2]1([C:15]([O:17][CH3:23])=[O:16])[C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][C:8]=2[C:9]2[C:14]1=[CH:13][CH:12]=[CH:11][CH:10]=2

Komponenten

5

Edukt 3

HCID 1118Sulfuric AcidHCID 10087FlurenolHCID 516892Sodium Bicarbonate

Produkt 1

HCID 267210Methyl 9-hydroxy-9H-fluorene-9-carboxylate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

50.4 g (0.223 mol) 9-hydroxy-9-fluorenecarboxylic acid are dissolved in 500 ml of methanol, combined with 5 ml (0.089 mol) conc. sulphuric acid and refluxed for 1 hour. After cooling 100 ml sodium hydrogen carbonate solution (about pH 8) are added, and the methanol is largely distilled off under reduced pressure. The residue remaining is extracted with dichloromethane and water, the organic phase is dried and evaporated to dryness.

Aufarbeitung

  1. temperaturerefluxed for 1 hour
  2. additionare added
  3. distillationthe methanol is largely distilled off under reduced pressure
  4. extractionThe residue remaining is extracted with dichloromethane and water
  5. customthe organic phase is dried
  6. customevaporated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-0c0f7af10541490f902dc8554975b448
Quelldatensatz
uspto-grants-2008_09
Patentnummer
US07429601B2

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