HRID4198

反应详情

EQUATION

反应方程式

HRID 4198 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 30.7 g (0.15 mole) of 2-chloroethylphenylsulfone and 69.5 g (0.375 mole) of potassium phthalimide in 600 ml of dimethylformamide was heated overnight at 85° C. The reaction mixture was stripped to dryness and the residue was partitioned between water and chloroform. The chloroform layer was dried and filtered and solvent was evaporated from the filtrate to give an oil which crystallized on standing. The solid was triturated with isopropyl ether and the mixture cooled under refrigeration. The solid was collected by filtration and dried and recrystallized from methanol-isopropyl ether to give white crystalline product, m.p. 186°-188° C., in 35.7% yield.

WORKUP

后处理

  1. customthe residue was partitioned between water and chloroform
  2. dry with materialThe chloroform layer was dried
  3. filtrationfiltered
  4. customsolvent was evaporated from the filtrate
  5. customto give an oil which
  6. customcrystallized
  7. customThe solid was triturated with isopropyl ether
  8. temperaturethe mixture cooled under refrigeration
  9. filtrationThe solid was collected by filtration
  10. customdried
  11. customrecrystallized from methanol-isopropyl ether
  12. customto give white crystalline product, m.p. 186°-188° C.