HRID2305002

反应详情

EQUATION

反应方程式

HRID 2305002 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

35.4 g of octafluorotoluene (0.15 mol) are dissolved in 400ml of dimethylformamide, the solution is cooled to 0øC using a cryostat, and a solution of 40 g of potassium 4-benzyloxycarbonylphenoxide (0.15 mol) in 300 ml of dimethylformamide is then added dropwise over the course of 2 hours. After 2hours at 0° C., the potassium salt has reacted. The dimethylformamide is then removed in a rotary evaporator, the residue is taken up in a little tetrahydrofuran, and the solution is filtered through a silica-gel column. The clear solution obtained is evaporated in a rotary evaporator until the reaction product precipitates out. The reaction product is then stirred in n-hexane, filtered off through a fluted filter and then dried for 48 hours under nitrogen at 40° C./10 mbar in a vacuum drying cabinet (yield: 95%).

WORKUP

后处理

  1. temperaturethe solution is cooled to 0øC
  2. customThe dimethylformamide is then removed in a rotary evaporator
  3. filtrationthe solution is filtered through a silica-gel column
  4. customThe clear solution obtained
  5. customis evaporated in a rotary evaporator until the reaction product
  6. customprecipitates out
  7. filtrationfiltered off through
  8. filtrationa fluted filter
  9. customdried for 48 hours under nitrogen at 40° C./10 mbar in a vacuum
  10. customdrying cabinet (yield: 95%)