HRID1293051

反应详情

EQUATION

反应方程式

HRID 1293051 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

(2R,3R,4R,5R)-4-(Acetyloxy)-2-[(acetyloxy)methyl]-5-(6-{[2,2-bis(4-methylphenyl)ethyl]amino}-2-cyano-9H-purin-9-yl)tetrahydro-3-furanyl acetate (Preparation 59) (837 mg, 1.33 mmol) was dissolved in a saturated solution of ammonia in ethanol (25 ml). 10% Palladium on carbon (168 mg) was added and the suspension was stirred under an atmosphere of hydrogen (414 kPa, 60 psi) for 16 hours. The reaction mixture was filtered through Arbocel (Trade Mark) and the filtrate was evaporated under reduced pressure. The residue was dissolved in methanol (100 ml) and sodium carbonate (100 mg) was added. The suspension was stirred at room temperature for 2 hours. The solvent was removed under reduced pressure and the residue was dissolved in a mixture of dichloromethane (15 ml) and water (15 ml). The dichloromethane layer was washed with water (15 ml) and saturated aqueous sodium chloride solution. The solvent was removed under reduced pressure. The residue was triturated with diethyl ether to give the title compound as a solid (340 mg).

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered through Arbocel (Trade Mark)
  2. customthe filtrate was evaporated under reduced pressure
  3. dissolutionThe residue was dissolved in methanol (100 ml)
  4. additionsodium carbonate (100 mg) was added
  5. stirringThe suspension was stirred at room temperature for 2 hours
  6. customThe solvent was removed under reduced pressure
  7. dissolutionthe residue was dissolved in a mixture of dichloromethane (15 ml) and water (15 ml)
  8. washThe dichloromethane layer was washed with water (15 ml) and saturated aqueous sodium chloride solution
  9. customThe solvent was removed under reduced pressure
  10. customThe residue was triturated with diethyl ether