HRID1168287

反应详情

EQUATION

反应方程式

HRID 1168287 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 6-[(2,2-diphenylethyl)amino]-N-[2-(1-piperidinyl)ethyl]-9-tetrahydro-2H-pyran-2-yl-9H-purine-2-carboxamide (Preparation 10) (420 mg, 0.76 mmol) in ethanol (20 ml) was treated with 2 M aqueous hydrochloric acid (0.9 ml). The mixture was heated under reflux for 30 minutes after which time a white precipitate had formed. The mixture was cooled to room temperature and the solvent was removed under reduced pressure. The residue was partitioned between dichloromethane and 10% weight by volume aqueous ammonia. The organic phase was separated, dried (anhydrous magnesium sulphate), filtered and evaporated under reduced pressure to afford the title compound as a white solid (319 mg).

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 30 minutes after which time a white precipitate
  3. customhad formed
  4. customthe solvent was removed under reduced pressure
  5. customThe residue was partitioned between dichloromethane and 10% weight by volume aqueous ammonia
  6. customThe organic phase was separated
  7. dry with materialdried (anhydrous magnesium sulphate)
  8. filtrationfiltered
  9. customevaporated under reduced pressure