反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of 5.0 g of 7-vinylimidazo[5,1-b]thiazole in 40 ml of ethanol and 8 ml of water was added 2.0 g of 10% Pd-C, and the mixture was stirred under the atmosphere of hydrogen at room temperature overnight. The catalyst was removed by filtration, and the filtrate was concentrated to a small volume. The concentrate was diluted with 10 ml of a saturated aqueous sodium hydrogen carbonate solution, and extracted with 100 ml of ethyl acetate. The organic layer was washed with aqueous saline and dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure. The residue thus obtained was purified by column chromatography on silica gel (dichloromethane:ethyl acetate=3:2) to give 1.27 g of 7-ethylimidazo[5,1-b]thiazole.
WORKUP
后处理
- customThe catalyst was removed by filtration
- concentrationthe filtrate was concentrated to a small volume
- additionThe concentrate was diluted with 10 ml of a saturated aqueous sodium hydrogen carbonate solution
- extractionextracted with 100 ml of ethyl acetate
- washThe organic layer was washed with aqueous saline
- dry with materialdried over anhydrous magnesium sulfate
- customthe solvent was removed under reduced pressure
- customThe residue thus obtained
- customwas purified by column chromatography on silica gel (dichloromethane:ethyl acetate=3:2)