HRID2304999

反应详情

EQUATION

反应方程式

HRID 2304999 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

33.8 g of pentafluoropyridine (0.2 mol) are dissolved in 500 ml of dimethylformamide, the solution is cooled to OC by means of a cryostat, and a solution of 53.3 g of potassium 4-benzyloxycarbonylphenoxide (0.2 mol) in 400 ml of dimethylformamide is then added dropwise over the course of 2 hours. After 24 hours 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 via a fluted filter and then dried for 48 hours under nitrogen at 40° C./10 mbar in a vacuum drying cabinet (yield: 91%).

WORKUP

后处理

  1. temperaturethe solution is cooled to OC by means of a cryostat
  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 via
  8. filtrationa fluted filter
  9. customdried for 48 hours under nitrogen at 40° C./10 mbar in a vacuum
  10. customdrying cabinet (yield: 91%)