HRID1582176
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
2-Mercaptothiazole (5.18 g), potassium carbonate (6.72 g) and 4-bromo-1,1,2-trifluorobutene-1 (9.21 g) are refluxed in acetonitrile (60 ml) in the presence of argon gas for 6 hours by heating. After the reaction mixture has reached room temperature, it is filtered and the solvent is distilled off. The residue is dissolved in dichloromethane and washed with 5% aqueous solution of sodium hydroxide and water in this order. It is dried over unhydrous sodium sulfate and purified by column chromatography (eluent: dichloromethane) to obtain 2-(3,4,4-trifluoro-3-butenyl-thio)thiazole (8.6 g) as pale yellow liquid (n20D 1.5200).
WORKUP
后处理
- temperatureby heating
- customhas reached room temperature
- filtrationit is filtered
- distillationthe solvent is distilled off
- dissolutionThe residue is dissolved in dichloromethane
- washwashed with 5% aqueous solution of sodium hydroxide and water in this order
- dry with materialIt is dried over unhydrous sodium sulfate
- custompurified by column chromatography (eluent: dichloromethane)