Reaktion #700177

ord-0305c9a0ec3341149eab85c971c58f87

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe catalyst was removed by filtration
  2. 2
    Sonstigethe filtrate was evaporated
  3. 3
    Sonstigeto afford a solid
  4. 4
    SonstigeThe solid was recrystallized from toluene
  5. 5
    Sonstigedried at 60° C.

Vorschrift

To 15.0 g (0.045 moles) of 5-{[3,5-bis(1,1-dimethylethyl)-4-hydroxyphenyl]} methylene-2,4-thiazolidinedione, in 375 ml of ethyl acetate, 3.0 g of 10% palladium on carbon was added. The mixture was heated at 80° C. in the presence of 50 psi (345 KPa) of hydrogen for 4.5 hours. An additional 3.0 g of 10% palladium on carbon was added and the mixture was again heated at 80° C. in the presence of 50 psi (345 KPa) of hydrogen for 2 hours. The catalyst was removed by filtration and the filtrate was evaporated to afford a solid. The solid was recrystallized from toluene and dried at 60° C. to obtain 8.93 g (59% yield) of subtitled compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06005142uspto-grants-1999_12