HRID1291355

反应详情

EQUATION

反应方程式

HRID 1291355 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3,5-dimethyl-2-mercaptoquinazolin-4-one (2.03 g, 9.74 mmol) in EtOH (30.0 ml)-THF (30.0 ml) was added 1N-aqueous sodium hydroxide solution (10.0 ml). Then, 4-(4-nitrobenzoyl)benzyl bromide (3.50 g, 10.9 mmol) was added and the mixture was stirred at room temperature overnight. The solvent was then distilled off and the residue was dissolved in ethyl acetate and washed with saturated aqueous NaCl solution. The organic layer was dried over MgSO4 and concentrated under reduced pressure. The residue was recrystallized from methanol to provide light-yellow needles.

WORKUP

后处理

  1. distillationThe solvent was then distilled off
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washwashed with saturated aqueous NaCl solution
  4. dry with materialThe organic layer was dried over MgSO4
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was recrystallized from methanol
  7. customto provide light-yellow needles