Reaktion #1012284

ord-44b05cb24fd24b80b36b277a428fe506

Reaktionsbedingungen

Temperatur
200°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeobtaining a mixture
  2. 2
    SonstigeThe reaction vessel was sealed
  3. 3
    Sonstigeto obtain a reaction mixture
  4. 4
    SonstigeThereafter, the obtained reaction mixture
  5. 5
    Temperaturwas cooled
  6. 6
    Filtrationfiltered
  7. 7
    WaschenThe obtained solid was washed with 20 parts by weight of 2-propanol
  8. 8
    SonstigeThe washing liquid recovered
  9. 9
    Waschenafter washing
  10. 10
    Sonstigethe filtrate obtained by filtration
  11. 11
    EinengenThe combined mixture was concentrated under reduced pressure

Vorschrift

Into a reaction vessel were charged 6.00 parts by weight of (3R)-1,1,3-trimethyl-4-aminoindane (optical purity of 96.5% ee) and 1.62 parts by weight of 5% palladium-carbon (STD-type, manufactured by N. E. Chemcat Corporation), thereby obtaining a mixture. The reaction vessel was sealed, the gas in the reaction vessel was replaced with nitrogen, and then the mixture was stirred at 200° C. for 7.5 hours to obtain a reaction mixture. Thereafter, the obtained reaction mixture was cooled and filtered. The obtained solid was washed with 20 parts by weight of 2-propanol. The washing liquid recovered after washing and the filtrate obtained by filtration were combined. The combined mixture was concentrated under reduced pressure to obtain 5.06 parts by weight of 1,1,3-trimethyl-4-aminoindane. The obtained 1,1,3-trimethyl-4-aminoindane had an optical purity of 3.3% ee and a recovery rate of 84.3%.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09284260B2uspto-grants-2016_03