HRID1291335
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
A solution of 3,5-dimethyl-2-mercapto-4(3H)-quinazolinone (1.03 g), 4,4'-bis (bromomethyl)benzophenone (1.75 g), 1-methyl-5-mercapto-1H-tetrazole (700 mg), and 1N-aqeuous sodium hydroxide solution (5.5 ml) in DMF (20 ml) 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 (603 mg).
WORKUP
后处理
- concentrationThis reaction mixture was concentrated
- dissolutionthe residue was dissolved in ethyl acetate
- washwashed with water
- customdried
- concentrationconcentrated
- customThe residue was purified by silica gel column chromatography (chloroform: methanol: aqueous ammonia=50:1:0.1)
- customcrystallized from methanol