تفاعل #2030970

ord-656b2e8d506c47bbbfb85672688a4e7d

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe reaction mixture was partitioned between ethyl acetate and water
  2. 2
    أخرىThe organic phase was separated
  3. 3
    غسيلwashed with hydrochloric acid (2N), brine
  4. 4
    تجفيفdried (MgSO4)
  5. 5
    أخرىevaporated to dryness
  6. 6
    أخرىThe crude product was triturated with ether
  7. 7
    ترشيحthe solid collected by filtration

الإجراء التجريبي

8-chloro-7-(2-propen-1-yl)-3,7-dihydro-1H-purine-2,6-dione (1.5 g, 6.64 mmol), sodium carbonate (844 mg, 7.9 mmol) and 4-bromo-1,1,1-trifluorobutane (1.39 g, 7.3 mmol) were stirred in dimethylformamide (25 ml, dry) for seven days. The reaction mixture was partitioned between ethyl acetate and water. The organic phase was separated and washed with hydrochloric acid (2N), brine, dried (MgSO4) and then evaporated to dryness. The crude product was triturated with ether and the solid collected by filtration to afford 8-chloro-7-(2-propen-1-yl)-3-(4,4,4-trifluorobutyl)-3,7-dihydro-1H-purine-2,6-dione as a white solid (1.23 g, 57%). m/z 337 [MH+].

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08394808B2uspto-grants-2013_03