تفاعل #1184829

ord-9da0aabc817a471d9ca88ff34cc418da

المذيبات

ظروف التفاعل

درجة الحرارة
50°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةthen cooled
  2. 2
    أخرىevaporated
  3. 3
    أخرىThe residue was partitioned between EtOAc (100 ml) and saturated aqueous sodium bicarbonate (50 ml)
  4. 4
    تجفيفThe organic phase was dried (MgSO4)
  5. 5
    ترشيحfiltered
  6. 6
    أخرىevaporated
  7. 7
    أخرىThe residue was triturated in a mixture of diethyl ether and cyclohexane
  8. 8
    ترشيحthe product filtered off
  9. 9
    أخرىdried

الإجراء التجريبي

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%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08143264B2uspto-grants-2012_03