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 a stirred solution of 9-benzyloxy-6-(2,3-dichlorobenzyl)-2-isopropyl-3,4-dihydro-2H-pyrazino[1,2-c]pyrimidine-1,8-dione (134) (70 mg, 0.095 mmol) in methanol (3 mL) was added concentrated HCl (3 mL) and the reaction mixture was stirred for 5 h at room temperature. After completion of the reaction, the mixture was evaporation and the residue was basified with saturated aqueous NaHCO3 solution. The mixture was extracted with 10% methanol in dichloromethane, the organic part was separated. The drying over sodium sulfate was conducted and concentration to get a crude product, which was washed with ether followed by pentene to get 6-(2,3-dichlorobenzyl)-9-hydroxy-2-isopropyl-3,4-dihydro-2H-pyrazino[1,2-c]pyrimidine-1,8-dione (135) (35 mg, 61.7%) as a brown colored solid.
WORKUP
后处理
- customAfter completion of the reaction
- customevaporation
- extractionThe mixture was extracted with 10% methanol in dichloromethane
- customthe organic part was separated
- concentrationconcentration
- customto get a crude product, which
- washwas washed with ether