HRID1354453
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 mixture of methyl 4-chloroformylbenzoate (1.17 g), 5-(4-t-butylphenyl)-1H-tetrazole (1.00 g) and pyridine (10 ml) was heated under reflux for 1 hr. After cooling, water was added to the mixture. The crystals were collected by filtration and dissolved in ethyl acetate. This solution was washed with 1 M hydrochloric acid, water and saturated brine, dried over anhydrous magnesium sulfate and concentrated. The residue was washed with cold hexane to give methyl 4-[5-(4-t-butylphenyl)-1,3,4-oxadiazol-2-yl]benzoate (1.51, yield 92%). Recrystallization from hexane-tetrahydrofuran gave colorless prism crystals. melting point: 210–211° C.
WORKUP
后处理
- temperaturewas heated
- temperatureunder reflux for 1 hr
- temperatureAfter cooling
- filtrationThe crystals were collected by filtration
- dissolutiondissolved in ethyl acetate
- washThis solution was washed with 1 M hydrochloric acid, water and saturated brine
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated
- washThe residue was washed with cold hexane