反応 #62403

反応方程式

sodium thiosulfate

5-fluoro-o-toluidine

N-bromosuccinimide

→

title compound

収率 102.1%

4-Bromo-5-fluoro-2-methylphenylamine

収率 102.1%

溶媒

dichloromethane

反応条件

後処理

1. 1
   その他the reaction solution was evaporated
2. 2
   workup.ADDITIONdiluted with ethyl acetate
3. 3
   洗浄The organic layer was washed successively with water and saturated brine
4. 4
   乾燥dried over anhydrous magnesium sulfate
5. 5
   その他Then the solvent was evaporated
6. 6
   洗浄the precipitated crystals were washed with diethyl ether

実験手順

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.

出典