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
Diphosphorus pentasulfide (846 mg) was added to 8.4 ml of formamide. The mixture was stirred at room temperature overnight. 7-Chloroacetylimidazo[5,1-b]thiazole (2.32 g) was added to the reaction solution. The mixture was stirred at room temperature for 15 hr. Water (20 ml) and 10 ml of dichloromethane were added thereto The mixture was adjusted to pH 8.8 by gradually adding a sodium hydrogencarbonate powder. Extraction was carried out six times with 50 ml of dichloromethane. The organic layer was dried over anhydrous magnesium sulfate. The solvent was removed by distillation under the reduced pressure. The residue was purified by column chromatography on silica gel (hexane ethyl acetate=1 2) to give 1.72 g of 7-(thiazol-4-yl)imidazo[5,1-b]thiazole.
WORKUP
后处理
- stirringThe mixture was stirred at room temperature for 15 hr
- extractionExtraction
- dry with materialThe organic layer was dried over anhydrous magnesium sulfate
- customThe solvent was removed by distillation under the reduced pressure
- customThe residue was purified by column chromatography on silica gel (hexane ethyl acetate=1 2)