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
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
To a solution of 8-(4-Benzyloxy-phenyl)-1-propyl-2-(3-trifluoromethyl-phenyl)-7-(2-trimethylsilanyl-ethoxymethyl)-1,7-dihydro-purin-6-one (0.217 g, 0.24 mmol) in DMF:water (2.5 ml), 10% Pd/C (0.120 g) and ammonium formate (0.431 g, 6.8 mmol) were added and refluxed at 80° C. for 2 hours. The mixture was cooled and filtered through celite bed, solvent was evaporated and the residue was diluted with water (10 ml), acidified with citric acid and extracted with ethyl acetate (3×10 ml). The organic layer was washed with brine (2×15 ml). It was dried over Na2SO4 and the solvent was evaporated to obtain off white solid of 8-(4-Hydroxy-phenyl)-1-propyl-2-(3-trifluoromethyl-phenyl)-7-(2-trimethylsilanyl-ethoxymethyl)-1,7-dihydro-purin-6-one (0.237 g, quantitative).
WORKUP
后处理
- temperatureThe mixture was cooled
- filtrationfiltered through celite bed, solvent
- customwas evaporated
- additionthe residue was diluted with water (10 ml)
- extractionextracted with ethyl acetate (3×10 ml)
- washThe organic layer was washed with brine (2×15 ml)
- dry with materialIt was dried over Na2SO4
- customthe solvent was evaporated