反応 #336951

反応方程式

7-allyl-3,7-dihydro-1H-purine-2,6-dione

sodium carbonate

1-iodopentane

→

desired product

収率 45.5%

7-Allyl-3-pentyl-3,7-dihydro-1H-purine-2,6-dione

収率 45.5%

溶媒

water

EtOAc

DMF

反応条件

後処理

1. 1
   抽出The aqueous layer was extracted with EtOAc three times
2. 2
   洗浄The combined organic layers were washed with brine
3. 3
   乾燥dried over Na2SO4
4. 4
   濃縮concentrated
5. 5
   workup.ADDITIONThe residue was treated with ether
6. 6
   その他the solid formed
7. 7
   ろ過was filtered

実験手順

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.

出典