HRID2288994

反应详情

EQUATION

反应方程式

HRID 2288994 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionare mixed together in a sealed tube
  2. temperatureThe mixture is cooled
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe crude material is purified by column chromatography (SiO2, 10% methanol: methylene chloride)
  6. customto afford an oil which
  7. customis triturated from 70% hexane