HRID2288994
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
CONDITIONS
反应条件
- 温度
- 150 °C
PROCEDURE
实验过程
1-(2-chloroethyl)-4-methoxybenzene (486 mg, 2.8 mmol), 4-(4-ethoxymethyl-5-phenyl-oxazol-2-yl)-piperidine hydrochloride (1 g, 2.2 mmol), prepared as in Intermediate 4, K2CO3 (393 mg, 2.85 mmol) and Nal (427 mg, 2.85 mmol) in ethanol are mixed together in a sealed tube and heated to 150° C. overnight. The mixture is cooled, filtered and concentrated. The crude material is purified by column chromatography (SiO2, 10% methanol: methylene chloride), followed by another column (SiO2, 15% methanol: ethyl acetate) to afford an oil which is triturated from 70% hexane; ether, 800 mg of the title compound is obtained.
WORKUP
后处理
- additionare mixed together in a sealed tube
- temperatureThe mixture is cooled
- filtrationfiltered
- concentrationconcentrated
- customThe crude material is purified by column chromatography (SiO2, 10% methanol: methylene chloride)
- customto afford an oil which
- customis triturated from 70% hexane