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 0.75 g (2.59 mmol) of 4-(4-(2-chloroethyl)phenyl)-2-aminothiazole hydrobromide, 0.69 g (2.59 mmol) of N-(3-trifluoromethylphenyl)piperazine hydrochloride, 1.08 ml (7.78 mmol) of triethylamine, 0.27 g (2.59 mmol) of sodium carbonate, 5 mg of sodium iodide, and 9.5 ml of ethanol. The reaction was heated at reflux, cooled, and taken up in ethyl acetate/water. The layers were separated, the ethyl acetate washed with brine, dried, and evaporated to give an oil. The oil was chromatographed on silica gel using ethyl acetate as eluent to give an oil. The oil was taken up in ethyl acetate/methanol, ether saturated with HCl was added, the precipitate filtered, washed with ether, and dried to give a white solid, 0.72 g (50%), m.p. 110°-115° C.
WORKUP
后处理
- customTo a 35 ml round-bottomed flask equipped with condenser and N2 inlet
- temperatureThe reaction was heated
- temperatureat reflux
- temperaturecooled
- customThe layers were separated
- washthe ethyl acetate washed with brine
- customdried
- customevaporated
- customto give an oil
- customThe oil was chromatographed on silica gel
- customto give an oil
- filtrationthe precipitate filtered
- washwashed with ether
- customdried
- customto give a white solid, 0.72 g (50%), m.p. 110°-115° C.