HRID2106797

反应详情

EQUATION

反应方程式

HRID 2106797 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 7.6 g of 2-chloro-3-bromo-5-(trifluoromethyl)pyridine, 6.2 ml of 25 percent sodium methoxide in methanol (0.027 mol), and 20 ml of anhydrous methanol was prepared and allowed to react at ambient temperature with stirring for 16 hours. The mixture was then poured onto ice and the resulting mixture extracted with ether. The ether extract was extracted with water, dried over sodium sulfate, and concentrated by evaporation under reduced pressure and the residue was purified by distillation under reduced pressure to obtain 4.1 g (65 percent of theory) of the title compound as a colorless oil boiling at 86°-88° C. at 21 mm pressure and having a refractive index at 19° C. of 1.4816. The proton nmr spectrum was consistent with the assigned structure.

WORKUP

后处理

  1. customwas prepared
  2. customto react at ambient temperature
  3. additionThe mixture was then poured onto ice
  4. extractionthe resulting mixture extracted with ether
  5. extractionThe ether extract
  6. extractionwas extracted with water
  7. dry with materialdried over sodium sulfate
  8. concentrationconcentrated by evaporation under reduced pressure
  9. distillationthe residue was purified by distillation under reduced pressure