HRID1870621

反应详情

EQUATION

反应方程式

HRID 1870621 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-10 °C

PROCEDURE

实验过程

37.6 g of decafluorobiphenyl (0.112 mol) are dissolved in 700 ml of dimethylformamide, and the solution is cooled to -10° C. by means of a cryostat, and a solution of 15 g of potassium 4-benzyloxycarbonylphenoxide (0.056 mol) in 300 ml of dimethylformamide is then added drop wise over the course of 2 hours. After 48 hours at -10° C., the potassium salt has reacted. The dimethylformamide is then removed in a rotary evaporator, and the residue is taken up in a little tetrahydrofuran and filtered via 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.

WORKUP

后处理

  1. customThe dimethylformamide is then removed in a rotary evaporator
  2. filtrationfiltered via a silica-gel column
  3. customThe clear solution obtained
  4. customis evaporated in a rotary evaporator until the reaction product
  5. customprecipitates out
  6. filtrationfiltered off via
  7. filtrationa fluted filter
  8. customdried for 48 hours under nitrogen at 40° C./10 mbar in a vacuum
  9. customdrying cabinet