反应 #62403

反应方程式

sodium thiosulfate

5-fluoro-o-toluidine

N-bromosuccinimide

→

title compound

收率 102.1%

4-Bromo-5-fluoro-2-methylphenylamine

收率 102.1%

溶剂

dichloromethane

反应条件

后处理

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

实验过程

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.

来源