HRID1293058

反应详情

EQUATION

反应方程式

HRID 1293058 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. filtrationThe precipitate was filtered off
  2. stirringstirred in dichloromethane (50 ml) for 10 minutes
  3. filtrationThe dichloromethane was filtered
  4. dry with materialdried over anhydrous magnesium sulphate
  5. customevaporated under reduced pressure
  6. customThe residue was purified by column chromatography on silica gel eluting with dichloromethane:methanol (98: 2 by volume)
  7. customThe solvent was removed under reduced pressure