HRID1291334
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), 2-mercaptothiazoline (600 mg), and 1N-sodium hydroxide/water (11 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 (hexane: ethyl acetate: chloroform=3:1:1) and crystallized from methanol to provide the title compound as colorless solid (489 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 (hexane: ethyl acetate: chloroform=3:1:1)
- customcrystallized from methanol