반응 #4294

ord-6acd335397af4423ab4dfd5c48ff189b

반응 방정식

O=S(=O)(CCCl)c1ccccc1
2-chloroethylphenylsulfone
O=C1NC(=O)c2ccccc21.[K]
potassium phthalimide
O=C1c2ccccc2C(=O)N1CCS(=O)(=O)c1ccccc1
2-[2-(Phenylsulfonyl)ethyl]-1H-isoindole-1,3-(2H)-dione
수율 35.7%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the residue was partitioned between water and chloroform
  2. 2
    건조The chloroform layer was dried
  3. 3
    여과filtered
  4. 4
    기타solvent was evaporated from the filtrate
  5. 5
    기타to give an oil which
  6. 6
    기타crystallized
  7. 7
    기타The solid was triturated with isopropyl ether
  8. 8
    온도the mixture cooled under refrigeration
  9. 9
    여과The solid was collected by filtration
  10. 10
    기타dried
  11. 11
    기타recrystallized from methanol-isopropyl ether
  12. 12
    기타to give white crystalline product, m.p. 186°-188° C.

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04724235uspto-grants-1988_02