Reaktion #451829

Reaktionsgleichung

triphenylphosphine

1,3-dibrompropane

dimethylamine

→

(3-dimethylaminopropyl)-triphenylphosphoniumbromide HBr

Ausbeute 88.6%

Lösungsmittel

xylene

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigefor 20 hours
2. 2
   Sonstigeat 20°-25° C.
3. 3
   Sonstigeis absorbed
4. 4
   Sonstigeafter removal of ethanol in a vacuum in 2-propanol
5. 5
   Sonstigeprecipitated
6. 6
   SonstigeAfter recrystallization from ethanol

Vorschrift

There is prepared from 50 g triphenylphosphine and 38.5 g 1,3-dibrompropane in 150 ml xylene by heating for 20 hours at 130° C. under nitrogen 80 g crystalline (3-bromopropyl)-triphenylphosphoniumbromide with a melting point of 226° C. This is stirred using a solution of 33 g (0.7M) dimethylamine in 200 ml ethanol for 20 hours at 20°-25° C.) The residue is absorbed after removal of ethanol in a vacuum in 2-propanol and precipitated using hydrogen bromide gas. After recrystallization from ethanol, 43 g (3-dimethylaminopropyl)-triphenylphosphoniumbromide HBr is obtained with a melting point of 279° C.

Quelle