HRID634676

反应详情

EQUATION

反应方程式

HRID 634676 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 7-benzyloxy-6-methoxy-3,4-dihydroquinazolin-4-one (5.0 g, mmol), (prepared as described for the starting material in Example 4), acetic anhydride (200 ml), sodium acetate (12 g), 10% palladium-on-charcoal catalyst (1.5 g) in toluene (100 ml) was stirred under an atmosphere of hydrogen for 3 hours. The mixture was filtered and the filtrate was evaporated. The residue was partitioned between a mixture of ethyl acetate (500 ml), methanol (20 ml) and water (300 ml). The organic phase was separated, dried (MgSO4) and the solvent removed by evaporation. The residue was triturated with hexane to give 7-acetoxy-6-methoxy-3,4-dihydroquinazolin-4-one (1.1 g, 27%).

WORKUP

后处理

  1. custom(prepared
  2. filtrationThe mixture was filtered
  3. customthe filtrate was evaporated
  4. customThe residue was partitioned between a mixture of ethyl acetate (500 ml), methanol (20 ml) and water (300 ml)
  5. customThe organic phase was separated
  6. dry with materialdried (MgSO4)
  7. customthe solvent removed by evaporation
  8. customThe residue was triturated with hexane