反应详情

To the solution of 21.8 g of methyl m-trifluoromethylphenylacetate in 450 ml of carbon tetrachloride a portion of 18.7 g of N-bromosuccinimide is added along with several drops of triethylamine and a pinch of azobisisobutyronitrile. The mixture is warmed to reflux with a 250 watt incandescent bulb and a precipitate is formed. Thereupon the remainder of N-bromosuccinimide is added, the light removed and the solution stirred for 3 hours. It is cooled in an ice bath and the solid formed removed by filtration. The filtrate is evaporated the residue dissolved in diethyl ether-water and the organic phase washed with aqueous sodium bicarbonate and water. It is dried, evaporated, the residue distilled and the fraction boiling at 85°-88°/0.4 mmHg collected, to yield the methyl α-bromo-m-trifluoromethylphenylacetate.

1. temperatureThe mixture is warmed
2. temperatureto reflux with a 250 watt incandescent bulb
3. customa precipitate is formed
4. customthe light removed
5. temperatureIt is cooled in an ice bath
6. customthe solid formed
7. customremoved by filtration
8. customThe filtrate is evaporated the residue
9. dissolutiondissolved in diethyl ether-water
10. washthe organic phase washed with aqueous sodium bicarbonate and water
11. customIt is dried
12. customevaporated
13. distillationthe residue distilled
14. customthe fraction boiling at 85°-88°/0.4 mmHg collected