Reaktion #11953

ord-b8d808e82a4642758ddd699886c22acc

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwhile cooling with ice
  2. 2
    Sonstigethe solvent was removed by distillation
  3. 3
    workup.DISSOLUTIONThe residue was dissolved in chloroform
  4. 4
    Waschenwashed with 1 mol/l aqueous solution of sodium hydroxide
  5. 5
    Trocknendried over anhydrous sodium sulfate
  6. 6
    SonstigeThe solvent was removed by distillation
  7. 7
    SonstigeThe residue was dried under reduced pressure

Vorschrift

Commercially available 4-methyl-1-naphthalenecarboxylic acid (250.6 mg) was dissolved in methanol (7.5 ml). Hydrogen chloride gas was blown into the solution for five minutes while cooling with ice. Then, the mixture was stirred for 19 hours at room temperature and the solvent was removed by distillation. The residue was dissolved in chloroform, washed with 1 mol/l aqueous solution of sodium hydroxide, and dried over anhydrous sodium sulfate. The solvent was removed by distillation. The residue was dried under reduced pressure to obtain the target compound (269.9 mg) as colorless oil.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07098215B2uspto-grants-2006_08