HRID1980231

反应详情

EQUATION

反应方程式

HRID 1980231 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

9.0 g. (0.05 moles) of α-cyano-β-phenyl-acrylic acid are suspended in 200 ml. of dichloromethane and 9.2 g. (0.05 moles) of pentafluorophenol and 10.02 g. (0.05 moles) of dicyclohexylcarbodiimide in 100 ml. dichloromethane are added. The mixture is heated for 5 hours under reflux, cooled, the precipitated dicyclohexyl urea is filtered off. The solution is washed with 20 ml. of 2n hydrochloric acid and three times with water, dried over magnesium sulfate, evaporated and the residual oily substance is recrystallized from petrolether.

WORKUP

后处理

  1. temperatureThe mixture is heated for 5 hours
  2. temperatureunder reflux
  3. temperaturecooled
  4. filtrationthe precipitated dicyclohexyl urea is filtered off
  5. washThe solution is washed with 20 ml
  6. dry with materialof 2n hydrochloric acid and three times with water, dried over magnesium sulfate
  7. customevaporated
  8. customthe residual oily substance is recrystallized from petrolether