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
CONDITIONS
反应条件
- 温度
- 90 °C
PROCEDURE
实验过程
Copper (I) cyanide was added to a solution of (2R,3R,4S,5S)-4-(benzoyloxy)-2-(6-{[2,2-bis(4-chlorophenyl)ethyl]amino}-2-iodo-9H-purin-9-yl)-5-[(ethylamino)carbonyl]tetrahydro-3-furanyl benzoate (440 mg, 0.494 mmol) (Preparation 67) in N′N′-dimethylformamide (10 ml). The reaction mixture was stirred at 90° C. overnight. The reaction mixture was poured into water (15 ml). The precipitate was filtered off and stirred in dichloromethane (50 ml) for 10 minutes. The dichloromethane was filtered, dried over anhydrous magnesium sulphate and evaporated under reduced pressure. The residue was purified by column chromatography on silica gel eluting with dichloromethane:methanol (98:2 by volume). The solvent was removed under reduced pressure to give the title compound (227 mg) as a foam.
WORKUP
后处理
- filtrationThe precipitate was filtered off
- stirringstirred in dichloromethane (50 ml) for 10 minutes
- filtrationThe dichloromethane was filtered
- dry with materialdried over anhydrous magnesium sulphate
- customevaporated under reduced pressure
- customThe residue was purified by column chromatography on silica gel eluting with dichloromethane:methanol (98:2 by volume)
- customThe solvent was removed under reduced pressure