تفاعل #336951

ord-992a00e7f7b1479cab0ce476acf75ff9

المذيبات

ظروف التفاعل

درجة الحرارة
45°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصThe aqueous layer was extracted with EtOAc three times
  2. 2
    غسيلThe combined organic layers were washed with brine
  3. 3
    تجفيفdried over Na2SO4
  4. 4
    تركيزconcentrated
  5. 5
    workup.ADDITIONThe residue was treated with ether
  6. 6
    أخرىthe solid formed
  7. 7
    ترشيحwas filtered

الإجراء التجريبي

A mixture of 7-allyl-3,7-dihydro-1H-purine-2,6-dione (10.0 g, 0.052 mol), sodium carbonate (8.3 g, 0.078 mol), and 1-iodopentane (12 g, 0.062 mol) in DMF (100 mL) was stirred at 45° C. for 2 days. The reaction mixture was diluted with water and EtOAc. The aqueous layer was extracted with EtOAc three times. The combined organic layers were washed with brine, dried over Na2SO4 and concentrated. The residue was treated with ether and the solid formed was filtered to provide the desired product as white solid (6.2 g, 45.4%). LCMS calculated for C13H19N4O2 (M+H): 263.2. found: 263.2.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07863285B2uspto-grants-2011_01