HRID487698
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 DL-α-(5-methoxybenzofuran-2-yl)carbonylamino-ε-caprolactam (0.2 g) and phosphorus pentasulfide (0.2 g) in pyridin (2 ml) was stirred under reflux for 6.5 hours. After being cooled, the resulting mixture was poured into ice-water, and extracted with ethyl acetate. The organic layer was washed with brine, dried over magnesium sulfate and concentrated under reduced pressure to give crude crystal, which was collected by filtration and washed with ethanol to give 2-(5-methoxybenzofuran-2-yl)-4,5,6,7-tetrahydro-8H-thiazolo[5,4-b]azepine (0.09 g).
WORKUP
后处理
- temperatureunder reflux for 6.5 hours
- temperatureAfter being cooled
- extractionextracted with ethyl acetate
- washThe organic layer was washed with brine
- dry with materialdried over magnesium sulfate
- concentrationconcentrated under reduced pressure
- customto give crude crystal, which
- filtrationwas collected by filtration
- washwashed with ethanol