HRID525840

反应详情

EQUATION

反应方程式

HRID 525840 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a 250 mL flask, 4.8 g of tetrachlorophthalonitrile, 3.98 g of methyl 4-hydroxybenzoate, 5 g of potassium carbonate (K2CO3), and 55 mL of acetonitrile are added, followed by heating for 12 hours while refluxing. After completion of the reaction, 30 mL of ethyl acetate is added and filtered to remove the solvent. To the obtained solid, a suitable amount of dichloromethane is added to dissolve the solid, followed by adding hexane for crystallization. The obtained solid is filtered and dried under vacuum to obtain a compound, methyl 4-(2,3,6-trichloro-4,5-dicyano-phenoxy)benzoate. The first step reaction may be represented by Reaction Scheme 1:

WORKUP

后处理

  1. temperatureby heating for 12 hours
  2. temperaturewhile refluxing
  3. additionis added
  4. filtrationfiltered
  5. customto remove the solvent
  6. additionTo the obtained solid, a suitable amount of dichloromethane is added
  7. dissolutionto dissolve the solid
  8. additionby adding hexane
  9. customfor crystallization
  10. filtrationThe obtained solid is filtered
  11. customdried under vacuum