Reaktion #93855

ord-901d954f193c43aca74ff7cd531634b3

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeis submitted to hydrogenation at atmospheric pressure and room temperature
  2. 2
    SonstigeAfter the absorption of 1200 ml of hydrogen the catalysts
  3. 3
    Sonstigeare removed by filtration
  4. 4
    EinengenThe solution is concentrated by evaporation in vacuo of most of the solvent
  5. 5
    Sonstigewhereafter the product crystallizes as white crystals melting at 152°-154° C

Vorschrift

A mixture of 205 g of 2,2-dimethyl-1-ethinyl-7-methoxy-3-(N-methyl-p-toluenesulphonamido)-1,2,3,4-tetrahydro-1-naphthol, 0.8 g of 0,5% palladium on calcium carbonate, 0.8 g 5% palladium on charcoal and 1000 ml of ethyl acetate is submitted to hydrogenation at atmospheric pressure and room temperature. After the absorption of 1200 ml of hydrogen the catalysts are removed by filtration. The solution is concentrated by evaporation in vacuo of most of the solvent, whereafter the product crystallizes as white crystals melting at 152°-154° C. Yield 95%.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04128548uspto-grants-1978_12