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 125 ml round-bottomed flask equipped with condenser and N2 inlet were added 2.39 g (7.5 mmol) of 4-(4-(2-chloroethyl)phenyl)-2-methylthiazole hydrobromide, 2.0 g (7.5 mmol) of N-(3-trifluoromethylphenyl)piperazine hydrochloride, 2.62 ml (15.0 mmol) of diisopropylethylamine, 1.59 g (15.0 mmol) of sodium carbonate, 5 mg of sodium iodide, and 50 ml of methylisobutylketone. The reaction was heated at reflux for 4.5 days, filtered hot to remove inorganic material, cooled, and the precipitate filtered and washed with ether and ethyl acetate. The solid was taken up in methylene chloride, hydrochloride gas bubbled through to precipitate the salt, and the resulting solid filtered, washed with methylene chloride, and dried to give a solid, m.p. 170°-175° C., 1.93 g (51%).
WORKUP
后处理
- customTo a 125 ml round-bottomed flask equipped with condenser and N2 inlet
- temperatureThe reaction was heated
- temperatureat reflux for 4.5 days
- filtrationfiltered hot
- customto remove inorganic material
- temperaturecooled
- filtrationthe precipitate filtered
- washwashed with ether and ethyl acetate
- custombubbled through
- customto precipitate the salt
- filtrationthe resulting solid filtered
- washwashed with methylene chloride
- customdried
- customto give a solid, m.p. 170°-175° C., 1.93 g (51%)