HRID429166
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of 3-(bromopentyloxy)benzamide (500 mg, 1.7 mmols), 6-chloropurine (270 mg, 1.7 mmols) and potassium carbonate (240 mg, 1.7 mmols) in DMF (7.5 ml) was stirred for two days at room temperature. The solvent was then removed under vacuum (0.001 mmHg) and the white solid (mixture of N7 and N9 isomers) was chromatographed (silica, 10% MeOH/CH2CI2) to give a single product (N9 isomer) as a glass. This was triturated with ether (=5 ml) to give a white solid which was recrystallised from ethyl acetate to give the product (120 mg, 0.33 mmols, 20% yield)
WORKUP
后处理
- customThe solvent was then removed under vacuum (0.001 mmHg)
- additionthe white solid (mixture of N7 and N9 isomers)
- customwas chromatographed (silica, 10% MeOH/CH2CI2)
- customto give a single product (N9 isomer) as a glass
- customThis was triturated with ether (=5 ml)
- customto give a white solid which
- customwas recrystallised from ethyl acetate