Reaktion #332136

ord-345845d3bbd14f6f9b0dbd5de8d93ac2

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeAfter completion of the reaction
  2. 2
    Filtrationthe palladium hydroxide carbon was filtered off
  3. 3
    workup.ADDITIONthe filtrate was mixed with 3 M hydrochloric acid
  4. 4
    Sonstigeseparated
  5. 5
    Extraktionextracted with methylene chloride
  6. 6
    EinengenThe organic layer was concentrated under reduced pressure

Vorschrift

25.4 g of 1-(2-azido-2-methylpropyl)-4-(trifluoromethyl)benzene was dissolved in 210 mL of ethyl acetate and mixed with 0.84 g of 20 wt % palladium hydroxide carbon. The atmosphere in the reaction vessel was replaced with hydrogen gas, and the reaction solution was stirred at room temperature for 18 hours. After completion of the reaction, the palladium hydroxide carbon was filtered off, and the filtrate was mixed with 3 M hydrochloric acid and separated. The aqueous layer was basified with 5 M sodium hydroxide and extracted with methylene chloride. The organic layer was concentrated under reduced pressure to give 4.27 g of the desired product as a brown liquid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08658686B2uspto-grants-2014_02