Acetic Anhydride → 1-Benzofuran-3-yl acetate

HRID 716727

Reaktionsgleichung

Reaktionsgleichung von HRID 716727
C([CH2:4][O:5][C:6]1[CH:14]=[CH:13][CH:12]=[CH:11][C:7]=1[C:8]([OH:10])=O)(O)=O.[C:15](OC(=O)C)(=[O:17])[CH3:16]>>[C:15]([O:10][C:8]1[C:7]2[CH:11]=[CH:12][CH:13]=[CH:14][C:6]=2[O:5][CH:4]=1)(=[O:17])[CH3:16]

Komponenten

3

Edukt 2

HCID 7918Acetic AnhydrideHCID 69461Benzoic acid, 2-(carboxymethoxy)-

Produkt 1

HCID 27696211-Benzofuran-3-yl acetateAusbeute 76 %

Reaktionsbedingungen

Temperatur
135 °C

Versuchsvorschrift

To acetic anhydride (300 mL) was added 2-(carboxymethoxy)benzoic acid (7) (100 g, 0.510 mol) at ambient temperature and heated to 130-140° C. The reaction temperature was maintained for 14-20 h under stirring. The progress of the reaction was monitored by the HPLC analysis. Upon completion of the reaction, the reaction mixture was cooled to 50-80° C., acetic anhydride was recovered at 50-80° C. at reduced pressure and the crude product was extracted with dichloromethane (500 mL). The dichloromethane layer was recovered completely to obtain the product meeting the desired specifications. Yield—76-85%.

Aufarbeitung

  1. temperatureThe reaction temperature was maintained for 14-20 h
  2. customUpon completion of the reaction
  3. temperaturethe reaction mixture was cooled to 50-80° C.
  4. customacetic anhydride was recovered at 50-80° C. at reduced pressure
  5. extractionthe crude product was extracted with dichloromethane (500 mL)
  6. customThe dichloromethane layer was recovered completely
  7. customto obtain the product

Quellen und Nachweise

ORD-Eintrag
ord-abcc828987ee480289539a370f4b9825
Quelldatensatz
uspto-grants-2015_11
Patentnummer
US09193698B2

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