HRID2169219

反应详情

EQUATION

反应方程式

HRID 2169219 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customAfter completion of the reaction
  2. customevaporation
  3. extractionThe mixture was extracted with 10% methanol in dichloromethane
  4. customthe organic part was separated
  5. concentrationconcentration
  6. customto get a crude product, which
  7. washwas washed with ether