반응 #1184829

ord-9da0aabc817a471d9ca88ff34cc418da

용매

반응 조건

온도
50°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도then cooled
  2. 2
    기타evaporated
  3. 3
    기타The residue was partitioned between EtOAc (100 ml) and saturated aqueous sodium bicarbonate (50 ml)
  4. 4
    건조The organic phase was dried (MgSO4)
  5. 5
    여과filtered
  6. 6
    기타evaporated
  7. 7
    기타The residue was triturated in a mixture of diethyl ether and cyclohexane
  8. 8
    여과the product filtered off
  9. 9
    기타dried

실험 절차

A solution of 8-chloro-7-(2-propen-1-yl)-3,7-dihydro-1H-purine-2,6-dione (2.0 g, 8.8 mmol) in DMF (20 ml) was treated with sodium carbonate (1.15 g, 10.8 mmol) and 4-bromo-1,1,1-trifluorobutane (1.86 g, 9.7 mmol). The mixture was stirred at 50° C. for 18 h then cooled and evaporated. The residue was partitioned between EtOAc (100 ml) and saturated aqueous sodium bicarbonate (50 ml). The organic phase was dried (MgSO4), filtered and evaporated. The residue was triturated in a mixture of diethyl ether and cyclohexane then the product filtered off and dried to yield the title compound as a white solid (1.18 g, 40%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08143264B2uspto-grants-2012_03