HRID420403

反应详情

EQUATION

反应方程式

HRID 420403 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-[3-(6-Bromo-hexyl)-2-(2-ethoxycarbonyl-ethyl)-phenoxy]-butyric acid ethyl ester (10.0 g, 21.2 mmol), pyridine N-oxide (10.06 g, 106 mmol), and sodium bicarbonate (10.0 g, 1 19 mmol) were heated at reflux with vigorous stirring in toluene (100 mL) for 24 hr. The mixture was cooled down and filtered. The filtrate was then evaporated under vacuo and the crude material was purified by column chromatography using 30% EtOAc-Hexane as eluant to give the title compound (7.0 g, 81%) as an oil. HR-MS-EI(+): calculated for C23H34O6 [M] 406.2350, found 406.2355.

WORKUP

后处理

  1. temperatureat reflux
  2. temperatureThe mixture was cooled down
  3. filtrationfiltered
  4. customThe filtrate was then evaporated under vacuo
  5. customthe crude material was purified by column chromatography