Reaktion #43942

Reaktionsgleichung

2-fluoro-4-hydroxybenzaldehyde

bromine

→

title compound

Ausbeute 81.2%

5-bromo-2-fluoro-4-hydroxybenzaldehyde

Ausbeute 81.2%

Lösungsmittel

acetic acid

acetic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   EinengenThe reaction mixture was concentrated under reduced pressure, brine
2. 2
   workup.ADDITIONwas added to the residue
3. 3
   Extraktionthe mixture was extracted with ethyl acetate
4. 4
   TrocknenThe extract was dried over anhydrous magnesium sulfate
5. 5
   Einengenconcentrated under reduced pressure
6. 6
   SonstigeThe residue was purified by silica gel column chromatography (ethyl acetate:hexane=5:95-40:60)

Vorschrift

To a solution of 2-fluoro-4-hydroxybenzaldehyde (2.16 g, 15.4 mmol) in acetic acid (70 mL) was added a solution of bromine (2.71 g, 17.0 mmol) in acetic acid (10 mL), and the mixture was stirred at 45° C. for 26 hr. The reaction mixture was concentrated under reduced pressure, brine was added to the residue, and the mixture was extracted with ethyl acetate. The extract was dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:hexane=5:95-40:60) to give the title compound (2.74 g, yield 81%) as colorless crystals.

Quelle