HRID1872404
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 suspension of 1-(4-n-Hexyloxybenzoyl)-2-(4-methoxycarbonylbenzoyl)hydrazine (1.00 g) in phosphorus oxychloride (5 ml) was refluxed for 1 hour. After cooling, the solution was concentrated under reduced pressure. The residue was poured into ice-water and extracted with dichloromethane. The organic layer was washed with water, brine and dried over magnesium sulfate. The solvents were removed under reduced pressure. The residue was triturated with acetonitrile, collected by filtration and dried under reduced pressure to give Methyl 4-[5-(4-n-hexyloxyphenyl)-1,3,4-oxadiazole-2-yl]benzoate (761 mg).
WORKUP
后处理
- temperaturewas refluxed for 1 hour
- temperatureAfter cooling
- concentrationthe solution was concentrated under reduced pressure
- additionThe residue was poured into ice-water
- extractionextracted with dichloromethane
- washThe organic layer was washed with water, brine
- dry with materialdried over magnesium sulfate
- customThe solvents were removed under reduced pressure
- customThe residue was triturated with acetonitrile
- filtrationcollected by filtration
- customdried under reduced pressure