HRID1291332

反应详情

EQUATION

反应方程式

HRID 1291332 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In DMF (20 ml) were dissolved 3,5-dimethyl-2-mercapto-4(3H)-quinazolinone (1.03 g), 4,4'-bis(bromomethyl) benzophenone (1.75 g), 1-(2-dimethylaminoethyl)-5-mercapto-1H-tetrazole (865 mg), and 1N-sodium hydroxide/water (11 ml) and the solution was stirred at room temperature for 30 minutes. This reaction mixture was concentrated and the residue was dissolved in ethyl acetate, washed with water, dried, and concentrated. The residue was purified by silica gel column chromatography (chloroform: methanol: aqueous ammonia=50:1:0.1) and crystallized from methanol to provide the title compound as colorless solid (337 mg).

WORKUP

后处理

  1. concentrationThis reaction mixture was concentrated
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washwashed with water
  4. customdried
  5. concentrationconcentrated
  6. customThe residue was purified by silica gel column chromatography (chloroform: methanol: aqueous ammonia=50:1:0.1)
  7. customcrystallized from methanol