反应 #954579

ord-bb79b63bca1945fb99b09014ed8b4eab

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他a strongly exothermic reaction
  2. 2
    温度by refluxing for two hours
  3. 3
    萃取extracted repeatedly with n-hexane
  4. 4
    洗涤The extracts are washed with water and saturated sodium chloride solution
  5. 5
    其他dried
  6. 6
    其他evaporated
  7. 7
    workup.DISTILLATIONthe residue is distilled

实验过程

A mixture of 18.2 g (0.09 mol) of 2-ethoxy-5-bromopyridine (can be obtained from 2,5-dibromopyridine and sodium methanolate in DMSO), 11.4 g (0.12 mol) of chlorodimethylsilane and 50 ml of anhydrous tetrahydrofuran (THF) is added dropwise to 2.4 g (0.10 mol) of magnesium turnings in 10 ml of anhydrous THF, a strongly exothermic reaction occurring. The reaction is completed by refluxing for two hours. The mixture is then poured into water and extracted repeatedly with n-hexane, The extracts are washed with water and saturated sodium chloride solution, dried and evaporated, and the residue is distilled. 7 g (43%) of 2-ethoxy-5-dimethylsilylpyridine are obtained as a colorless oil of boiling point 7=140°-150° C.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04775664uspto-grants-1988_10