Reaktion #55339
ord-ac795e5570e145a788b92da318c90f4b
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1EinengenThe reaction mixture was concentrated and to the concentrate
- 2workup.ADDITIONwas added 2N-NaOH solution
- 3ExtraktionThe product was extracted with ether
- 4Waschenwashed well with saturated sodium chloride solution
- 5Trocknendried over anhydrous sodium sulfate
- 6workup.ADDITIONTo the ether solution was added 20% ethanolic hydrogen chloride
- 7Sonstigeto yield white crystals
- 8SonstigeRecrystallization 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.