HRID1727366
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 suspension of 5-(2-chloromethyl-4-pyridyl)-2-ethyl-4-(3-methylphenyl)-1,3-thiazole (0.40 g, 1.2 mmol), potassium cyanide (0.095 g, 1.5 mmol), 18-crown-6 (0.14 g, 0.51 mmol) in acetonitrile (5 mL) was heated under reflux for 6 hours. After cooling, an aqueous potassium carbonate solution was added, and extracted with ethyl acetate. The extracts were washed with brine, then, dried, and concentrated. The residue was purified by silica gel column chromatography (hexane-ethyl acetate=2:1). The resulting crystal was washed with hexane-isopropyl ether to obtain a title compound (0.19 g, 48%).
WORKUP
后处理
- temperaturewas heated
- temperatureunder reflux for 6 hours
- temperatureAfter cooling
- extractionextracted with ethyl acetate
- washThe extracts were washed with brine
- customdried
- concentrationconcentrated
- customThe residue was purified by silica gel column chromatography (hexane-ethyl acetate=2:1)
- washThe resulting crystal was washed with hexane-isopropyl ether