反应 #63057

ord-d7d0eebacced4eeb9401093813d6f3e1

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.STIRRINGthe mixture stirred at 70° for 48 hours
  2. 2
    温度The reaction mixture was cooled
  3. 3
    过滤filtered
  4. 4
    workup.STIRRINGthe residue stirred with N aqueous acetic acid
  5. 5
    其他the undissolved solid collected

实验过程

A mixture of 4-amino-2-(4-phthalimidobutylthio)pyrimidine (0.49 g.), acetonitrile (5 ml.) and 2,2,2-trifluoroethylisothiocyanate (0.28 g.) was stirred at 70° for 48 hours. A further 0.28 g. of 2,2,2-trifluoroethylisothiocyanate was added and the mixture stirred at 70° for 48 hours. The reaction mixture was cooled and filtered, the residue stirred with N aqueous acetic acid and the undissolved solid collected to give 4-[3-(2,2,2-trifluoroethyl)thioureido]-2-(4-phthalimidobutylthio)pyrimidine (0.49 g.), m.p. 201°-202° after recrystallisation from a mixture of ethanol and dimethylformamide.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04762932uspto-grants-1988_08