反応 #336944

ord-95f15adcd3274c0687acf6b809a83c71

反応条件

温度
40°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出The aqueous layer was extracted with EtOAc twice
  2. 2
    その他The combined organic layers were dried
  3. 3
    ろ過filtered
  4. 4
    濃縮concentrated
  5. 5
    その他The resulting white solid was collected
  6. 6
    その他dried in vacuum oven at 50° C. for 18 h

実験手順

7-Benzyl-3,7-dihydro-1H-purine-2,6-dione (5.0 g, 21 mmol) was mixed with sodium carbonate (3.3 g, 31 mmol) and 1-iodopentane (4.0 mL, 31 mmol) in DMF (60 mL). After being stirred at 40° C. for 18 h, the reaction mixture was diluted with water and EtOAc. The aqueous layer was extracted with EtOAc twice. The combined organic layers were dried, filtered and concentrated. The resulting white solid was collected and dried in vacuum oven at 50° C. for 18 h to provide the desired product (2.84 g, 44% yield). LCMS calculated for C17H21N4O2(M+H): 313.2. found: 313.2.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07863285B2uspto-grants-2011_01