HRID1168287
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 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
- temperatureThe mixture was heated
- temperatureunder reflux for 30 minutes after which time a white precipitate
- customhad formed
- customthe solvent was removed under reduced pressure
- customThe residue was partitioned between dichloromethane and 10% weight by volume aqueous ammonia
- customThe organic phase was separated
- dry with materialdried (anhydrous magnesium sulphate)
- filtrationfiltered
- customevaporated under reduced pressure