Reaktion #362013

Reaktionsgleichung

phosphorus tribromide

2,3,5-trichlorophenylmethanol

→

2,3,5-trichlorophenylmethyl bromide

Lösungsmittel

toluene

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONUpon completion of addition
2. 2
   EinengenThe reaction mixture was then concentrated under reduced pressure to a residue
3. 3
   workup.DISSOLUTIONThe residue was dissolved in ethyl acetate
4. 4
   Waschenwashed with three portions of water
5. 5
   TrocknenThe organic layer was dried with sodium sulfate
6. 6
   Filtrationfiltered
7. 7
   EinengenThe filtrate was concentrated under reduced pressure

Vorschrift

A solution of 7.6 grams (0.028 mole) of phosphorus tribromide in 200 mL of toluene was stirred, and 17.0 grams (0.080 mole) of 2,3,5-trichlorophenylmethanol was washed into the reaction vessel with about 5 mL of toluene. Upon completion of addition, the reaction mixture was stirred at ambient temperature for about 16 hours. The reaction mixture was then concentrated under reduced pressure to a residue. The residue was dissolved in ethyl acetate and washed with three portions of water. The organic layer was dried with sodium sulfate and filtered. The filtrate was concentrated under reduced pressure, yielding 21.2 grams of 2,3,5-trichlorophenylmethyl bromide. The NMR spectrum was consistent with the proposed structure.

Quelle