Reaktion #705369

Reaktionsgleichung

acrylic acid

sodium dithionite

sodium bicarbonate

dibromodifluoromethane

→

oil

4-bromo-4,4-difluorobutanoic Acid

Lösungsmittel

water

acetonitrile

ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.DISSOLUTIONgradually dissolving
2. 2
   Sonstigeconsumption of acrylic acid
3. 3
   SonstigeThe organic phase was separated
4. 4
   Trocknendried over magnesium sulfate
5. 5
   Filtrationfiltered
6. 6
   Sonstigeevaporated under reduced pressure
7. 7
   Sonstigeto give a pale yellow oil with a small amount of a white solid
8. 8
   Filtrationfiltered
9. 9
   Sonstigesolvent evaporated under reduced pressure

Vorschrift

To a stirred solution of acrylic acid (1.44 g) and acetonitrile (80 cm3) was added sodium dithionite (4.18 g), sodium bicarbonate (2.01 g), water (20 cm3) and finally dibromodifluoromethane (5 cm3). The biphasic mixture was stirred at the ambient temperature with the inorganic salts gradually dissolving. GC analysis after 4 hours indicated complete consumption of acrylic acid. The aqueous phase was saturated with solid sodium chloride. The organic phase was separated, dried over magnesium sulfate, filtered and evaporated under reduced pressure to give a pale yellow oil with a small amount of a white solid. This mixture was taken up in ethyl acetate, filtered and solvent evaporated under reduced pressure to give a pale yellow oil (2.54 g). 1H NMR (DMSO-d6): δ 2.45(2H,t); 2.65(H,m).

Quelle