Реакция #4294

ord-6acd335397af4423ab4dfd5c48ff189b

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеthe residue was partitioned between water and chloroform
  2. 2
    СушкаThe chloroform layer was dried
  3. 3
    Фильтрацияfiltered
  4. 4
    Другоеsolvent was evaporated from the filtrate
  5. 5
    Другоеto give an oil which
  6. 6
    Другоеcrystallized
  7. 7
    ДругоеThe solid was triturated with isopropyl ether
  8. 8
    Температураthe mixture cooled under refrigeration
  9. 9
    ФильтрацияThe solid was collected by filtration
  10. 10
    Другоеdried
  11. 11
    Другоеrecrystallized from methanol-isopropyl ether
  12. 12
    Другоеto give white crystalline product, m.p. 186°-188° C.

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04724235uspto-grants-1988_02