反应 #2897

ord-ea8d9c1fc5de4b569364ab4d8c41abcc

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度The mixture was heated
  2. 2
    温度under reflux for 45 minutes
  3. 3
    温度cooled
  4. 4
    温度The mixture was heated
  5. 5
    温度under reflux for 4 hours
  6. 6
    workup.WAITleft
  7. 7
    其他Evaporation and crystallisation of the residue from dichloromethane

实验过程

Hydroxy(tosyloxy)iodobenzene (78.5 g) was added to a solution of 1,1,1-trifluoropentane-2,4-dione in acetonitrile (500 ml). The mixture was heated under reflux for 45 minutes, then cooled, and thiourea (15.2 g) was added. The mixture was heated under reflux for 4 hours and then left to stand overnight. Evaporation and crystallisation of the residue from dichloromethane gave the title compound.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05731335uspto-grants-1998_03