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
To a 35 ml round-bottomed flask equipped with condenser and N2 inlet were added 3.19 g (10 mmol) of 4-(4-(2-chloroethyl)phenyl)-2-aminothiazole hydrobromide, 2.12 g (10 mmol) of N-(1-naphthyl)piperazine, 2.79 ml (20 mmol) of triethylamine, 1.06 g (10 mmol) of sodium carbonate, 2 mg of sodium iodide, and 25 ml of ethanol. The reaction was heated at reflux for 5 days, cooled, and the precipitate filtered, and washed with ethanol and water. The orange solid was chromatographed on silica gel using ethyl acetate/methylene chloride as eluent to give a white solid. The solid was taken up in ethyl acetate/methanol, ether saturated with HCl added, the precipitate filtered, washed with ether, and dried to give a white solid, 1.61 g (31%), m.p. 274°-277° C.
WORKUP
后处理
- customTo a 35 ml round-bottomed flask equipped with condenser and N2 inlet
- temperatureThe reaction was heated
- temperatureat reflux for 5 days
- temperaturecooled
- filtrationthe precipitate filtered
- washwashed with ethanol and water
- customThe orange solid was chromatographed on silica gel
- customto give a white solid
- filtrationthe precipitate filtered
- washwashed with ether
- customdried
- customto give a white solid, 1.61 g (31%), m.p. 274°-277° C.