تفاعل #62403

معادلة التفاعل

sodium thiosulfate

5-fluoro-o-toluidine

N-bromosuccinimide

→

title compound

المردود 102.1%

4-Bromo-5-fluoro-2-methylphenylamine

المردود 102.1%

المذيبات

dichloromethane

ظروف التفاعل

المعالجة

1. 1
   أخرىthe reaction solution was evaporated
2. 2
   workup.ADDITIONdiluted with ethyl acetate
3. 3
   غسيلThe organic layer was washed successively with water and saturated brine
4. 4
   تجفيفdried over anhydrous magnesium sulfate
5. 5
   أخرىThen the solvent was evaporated
6. 6
   غسيلthe precipitated crystals were washed with diethyl ether

الإجراء التجريبي

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.

المصدر