HRID1060549
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 5) (420 mg, 0.76 mmol) in ethanol (20 ml) was treated with hydrochloric acid (2 M, 0.9 ml). The mixture was heated at 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 over 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
- temperatureat 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 over anhydrous magnesium sulphate
- filtrationfiltered
- customevaporated under reduced pressure