Reaktion #55339

ord-ac795e5570e145a788b92da318c90f4b

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    EinengenThe reaction mixture was concentrated and to the concentrate
  2. 2
    workup.ADDITIONwas added 2N-NaOH solution
  3. 3
    ExtraktionThe product was extracted with ether
  4. 4
    Waschenwashed well with saturated sodium chloride solution
  5. 5
    Trocknendried over anhydrous sodium sulfate
  6. 6
    workup.ADDITIONTo the ether solution was added 20% ethanolic hydrogen chloride
  7. 7
    Sonstigeto yield white crystals
  8. 8
    SonstigeRecrystallization from ethanol-ether

Vorschrift

A solution of 3.0 g of 2-(4-bromobutoxy)-2'-chlorobibenzyl in 15 ml of 50% aqueous dimethylamine solution and 15 ml of tetrahydrofuran was stirred at room temperature for 5 hours. The reaction mixture was concentrated and to the concentrate was added 2N-NaOH solution. The product was extracted with ether, washed well with saturated sodium chloride solution and then dried over anhydrous sodium sulfate. To the ether solution was added 20% ethanolic hydrogen chloride to yield white crystals. Recrystallization from ethanol-ether gave 2.8 g (93% yield) of 2-(4-dimethylaminobutoxy)-2'-chlorobibenzyl hydrochloride, m. p. 122°-123° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04220603uspto-grants-1980_09