Reaktion #4063

Reaktionsgleichung

1-acetyl-4-(2,5-difluorobenzoyl)piperidine

bromine

water

→

1-Acetyl-4-(2,5-difluorobenzoyl)-4-bromopiperidine

Lösungsmittel

ethyl acetate

acetic acid

acetic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeremained between 10°-12° C
2. 2
   Extraktionextracted twice with ethyl acetate
3. 3
   Sonstigethe solvent evaporated
4. 4
   Sonstigeto provide an oil
5. 5
   Waschenwashed with saturated sodium bicarbonate solution
6. 6
   Trocknendried over anhydrous magnesium sulfate
7. 7
   Filtrationfiltered
8. 8
   Sonstigethe solvent evaporated
9. 9
   Sonstigeto provide product as an oil

Vorschrift

To a stirred solution of 11.2 g of 1-acetyl-4-(2,5-difluorobenzoyl)piperidine in 225 ml of glacial acetic acid was added dropwise over 0.5 hr a solution of 13.5 ml (42.1 g) of bromine in 115 ml of glacial acetic acid at a rate such that the temperature remained between 10°-12° C. The mixture was stirred for an additional 10-15 mins, poured into water, extracted twice with ethyl acetate, and the solvent evaporated to provide an oil. The oil was dissolved in ethyl acetate, washed with saturated sodium bicarbonate solution, dried over anhydrous magnesium sulfate, filtered, and the solvent evaporated to provide product as an oil.

Quelle