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
To the stirred solution of 9-benzyloxy-2-isopropyl-6-(1-phenyl-cyclohexylmethyl)-3,4-dihydro-2H-pyrazino[1,2-c]pyrimidine-1,8-dione (259) (0.18 g, 0.37 mmol) in methanol (5.0 mL) was added concentrated HCl (5.0 mL) and the reaction mixture was stirred at room temperature for 3 h. After completion of the reaction, the solvent was reduced and the crude product was extracted with 10% methanol in dichloromethane. The organic part was washed with saturated NaHCO3 solution, separated and dried over Na2SO4. After evaporation, the crude product was purified by nor mal silica gel column chromatography (using 3% methanol in dichloromethane) to get 9-hydroxy-2-isopropyl-6-(1-phenyl-cyclohexylmethyl)-3,4-dihydro-2H-pyrazino[1,2-c]pyrimidine-1,8-dione (260) (70.0 mg, 48.0%) as a white solid.
WORKUP
后处理
- customAfter completion of the reaction
- extractionthe crude product was extracted with 10% methanol in dichloromethane
- washThe organic part was washed with saturated NaHCO3 solution
- customseparated
- dry with materialdried over Na2SO4
- customAfter evaporation
- customthe crude product was purified by nor mal silica gel column chromatography (using 3% methanol in dichloromethane)