HRID381232
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
5-Acetyl-2,3-dichloropyridine (24.5 g, 0.129 mol) was slurried in t-butanol (200 mL) and sodium methanethiolate (10 g, 0.143 mol) was added. The mixture was heated under reflux conditions for two hours, cooled to room temperature, and diluted with water (200 mL) and ether (150 mL). This was separated and the aqueous phase extracted with ether (50 mL). The combined organic extracts were washed with water (100 mL) and saturated sodium chloride solution (100 mL), dried over anhydrous sodium sulphate, and evaporated to dryness to give the desired product (24.1 g, 94%) as a pale, low melting solid.
WORKUP
后处理
- temperatureThe mixture was heated under reflux conditions for two hours
- customThis was separated
- extractionthe aqueous phase extracted with ether (50 mL)
- washThe combined organic extracts were washed with water (100 mL) and saturated sodium chloride solution (100 mL)
- dry with materialdried over anhydrous sodium sulphate
- customevaporated to dryness