Reaktion #1686166

ord-f94280474b7f4fe2a10aff68aa6ba646

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas heated 1 hour
  2. 2
    Temperaturat reflux
  3. 3
    Waschenwashed with diethyl ether (2×)
  4. 4
    workup.ADDITIONtreated with concentrated hydrochloric acid
  5. 5
    Temperaturcooled in an ice-bath
  6. 6
    SonstigeThe solids were collected
  7. 7
    Waschenwashed with water (2×)
  8. 8
    Sonstigedried under vacuum at 70° C.

Vorschrift

A mixture of methyl 6-methoxy-1,3-benzodioxole-5-carboxylate (3 g, 14 mmol), prepared as in Example 1, 20% sodium hydroxide (50 mL) and ethanol (25 mL) was heated 1 hour at reflux and then diluted with water, washed with diethyl ether (2×), treated with concentrated hydrochloric acid and cooled in an ice-bath. The solids were collected, washed with water (2×) and dried under vacuum at 70° C. to give 6-methoxy-1,3-benzodioxole-5-carboxylic acid (2.3 g, 12 mmol), m.p. 151° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05739336uspto-grants-1998_04