Reaktion #62403

Reaktionsgleichung

sodium thiosulfate

5-fluoro-o-toluidine

N-bromosuccinimide

→

title compound

Ausbeute 102.1%

4-Bromo-5-fluoro-2-methylphenylamine

Ausbeute 102.1%

Lösungsmittel

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe reaction solution was evaporated
2. 2
   workup.ADDITIONdiluted with ethyl acetate
3. 3
   WaschenThe organic layer was washed successively with water and saturated brine
4. 4
   Trocknendried over anhydrous magnesium sulfate
5. 5
   SonstigeThen the solvent was evaporated
6. 6
   Waschenthe precipitated crystals were washed with diethyl ether

Vorschrift

To a solution of 49.0 g of 5-fluoro-o-toluidine in 600 mL of dichloromethane was added 69.7 g of N-bromosuccinimide at 0° C., and stirred at this temperature for an hour. Then sodium thiosulfate aqueous solution was added, and the reaction solution was evaporated and diluted with ethyl acetate. The organic layer was washed successively with water and saturated brine and dried over anhydrous magnesium sulfate. Then the solvent was evaporated, and the precipitated crystals were washed with diethyl ether:n-hexane=1:10, to afford 81.6 g of the title compound as colorless crystals.

Quelle