HRID443448

反应详情

EQUATION

反应方程式

HRID 443448 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

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 reminder 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.

WORKUP

后处理

  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