HRID480180

反应详情

EQUATION

反应方程式

HRID 480180 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of (2R, 5S)-2-chloro-1-[4-(4-fluoro-benzyl)-2,5-dimethyl-piperazin-1-yl]-ethanone (2.75 g, 9.2 mmol) in butanone (50 ml) was added methyl 5-chloro-2-hydroxybenzoate (1.55 g, 9.2 mmol), potassium carbonate (2.54 g, 18.4 mmol) and potassium iodide (1.52 g, 9.2 mmol). The resulting mixture was stirred at reflux for 6 hours. The reaction was then cooled, diluted with ethyl acetate, and washed with brine. The organics were dried over magnesium sulfate, filtered and concentrated in vacuo to give an orange oil. Chromatography on silica gel gave the title compound (4.1 g, 100% yield).

WORKUP

后处理

  1. temperatureat reflux for 6 hours
  2. temperatureThe reaction was then cooled
  3. washwashed with brine
  4. dry with materialThe organics were dried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customto give an orange oil