Reaktion #45796

Reaktionsgleichung

4-Fluoro-2-hydroxybenzoic acid

bromine

→

compound

Ausbeute 93.0%

5-Bromo-4-fluoro-2-hydroxybenzoic acid

Ausbeute 93.0%

Lösungsmittel

acetic acid

acetic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwas gradually dropwise added at room temperature (1 hour)
2. 2
   Temperaturthis was cooled to room temperature
3. 3
   SonstigeThe reaction liquid
4. 4
   Sonstigewas dried to solidness under reduced pressure
5. 5
   workup.DISSOLUTIONthe residue was dissolved in methanol (100 ml)
6. 6
   workup.ADDITIONthis was poured into water (600 ml)
7. 7
   workup.STIRRINGAfter stirring at room temperature for 15 minutes
8. 8
   Waschenthe precipitated crystal was washed
9. 9
   Filtrationcollected by filtration
10. 10
    Sonstigedried

Vorschrift

4-Fluoro-2-hydroxybenzoic acid (29.01 g, 0.186 mol) was dissolved in acetic acid (290 ml), then a solution of bromine (31.18 g, 0.195 mol) dissolved in acetic acid (15 ml) was gradually dropwise added at room temperature (1 hour). After stirred at 60° C. for 24 hours, this was cooled to room temperature. The reaction liquid was dried to solidness under reduced pressure, the residue was dissolved in methanol (100 ml), and this was poured into water (600 ml). After stirring at room temperature for 15 minutes, the precipitated crystal was washed and collected by filtration, and dried to obtain the entitled compound (35.36 g, 93%) as a colorless solid.

Quelle