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
To a mixture of 3-mercapto-1H-1,2,4-triazole (1.15 g) and N,N-dimethylformamide (15 ml) was added 60% sodium hydride (450 mg). After foaming was completed, N-chlorosuccinimide in small portions was added to the mixture on an ice bath, and stirred at this temperature for 15 minutes. 2-methylimidazo[1,2-a]pyridine (1.0 g) was then added, and the reaction mixture was heated and stirred at room temperature for 1 hour, and then for 3 hours on an oil bath at 70° C. The reaction solution was concentrated under reduced pressure. The residue was washed twice with diethyl ether, and methanol was added to the residue to remove undissolved materials. The filtrate was concentrated, and then crystals precipitated by the addition of water were collected by filtration, washed with water, followed by diethyl ether, and dried to yield the title compound (480 mg).
WORKUP
后处理
- temperaturethe reaction mixture was heated
- stirringstirred at room temperature for 1 hour
- waitfor 3 hours on an oil bath at 70° C
- concentrationThe reaction solution was concentrated under reduced pressure
- washThe residue was washed twice with diethyl ether, and methanol
- additionwas added to the residue
- customto remove undissolved materials
- concentrationThe filtrate was concentrated
- customcrystals precipitated by the addition of water
- filtrationwere collected by filtration
- washwashed with water
- customdried