Reaktion #88209

Reaktionsgleichung

water

4-bromo-2,6-difluoroaniline

AcOH

H2O

AcOH

H2O

→

desired product

5-Bromo-1,3-difluoro-2-nitro-benzene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionextracted with Et2O
2. 2
   Sonstigeobtained from another reaction
3. 3
   EinengenThe mixture was concentrated
4. 4
   SonstigeA precipitate was formed
5. 5
   Sonstigeseparated by filtration
6. 6
   EinengenThe filtrate was concentrated

Vorschrift

A solution of 4-bromo-2,6-difluoroaniline (240 mmol) in AcOH (150 mL) was added dropwise to a suspension of NaBO3.4 H2O (325 mmol) in AcOH (450 mL) at 70° C. during 30 min. Another 2080 mmol of NaBO3.4 H2O were added over 5 h to the mixture. During this period the mixture was stirred at 70° C. The mixture was poured into water and extracted with Et2O. The organic layer was combined with another Et2O solution obtained from another reaction using the same conditions described above. The mixture was concentrated. A precipitate was formed and separated by filtration. The filtrate was concentrated to afford the desired product after flash column chromatography (SiO2, petroleum ether).

Quelle