反应 #1904042

ord-3e4f134a9bff4b51980c50faa3c02415

溶剂

反应条件

温度
30°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他A solution formed
  2. 2
    温度refluxed for two hours
  3. 3
    workup.STIRRINGthe mixture was stirred at −20° C. for five hours
  4. 4
    workup.DISTILLATIONThe solvent was distilled off under a reduced pressure
  5. 5
    workup.DISSOLUTIONthe remaining solid was dissolved into dichloromethane
  6. 6
    洗涤washed with water twice
  7. 7
    干燥The organic layer was dried over anhydride MgSO4
  8. 8
    workup.DISTILLATIONthe solvent was distilled off

实验过程

A solution formed by dissolving 4-bromostyrene (18.3 g, 0.1 mol) and magnesium (2.64 g, 0.11 mol) into THF (200 mL) was stirred at 30° C. for two hours, and then, refluxed for two hours. This solution was added to a solution of cyanuric chloride (21.58 g, 0.120 mol) into THF (200 mL) at −20° C., and the mixture was stirred at −20° C. for five hours. The solvent was distilled off under a reduced pressure, the remaining solid was dissolved into dichloromethane and washed with water twice. The organic layer was dried over anhydride MgSO4, and the solvent was distilled off.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07597980B2uspto-grants-2009_10