HRID1872836

反应详情

EQUATION

反应方程式

HRID 1872836 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of 2-(2-methoxy-phenoxy)acetonitrile (5 g, 31 mmol) in anhydrous ethyl ether (100 ml) was added lithium aluminum hydride (1.6 g, 40 mmol) portionwise. The reaction mixture was heated to reflux for 3 hours and then cooled to 0° C. The reaction was quenched with 1N hydrochloric acid and diluted with water (PH=1, aqueous layer). The mixture was extracted with ethyl acetate (3×150 ml), neutralized with 50% sodium hydroxide to pH>10, and extracted again with more ethyl acetate (3×100 ml). The combined organic layers were washed with brine (3×150 ml), dried over anhydrous sodium sulfate and filtered. The solvent was removed under vacuum to afford 2.85 g (56%) of product as an oil; MS EI m/e 167 (M+).

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 3 hours
  3. customThe reaction was quenched with 1N hydrochloric acid
  4. additiondiluted with water (PH=1, aqueous layer)
  5. extractionThe mixture was extracted with ethyl acetate (3×150 ml)
  6. extractionextracted again with more ethyl acetate (3×100 ml)
  7. washThe combined organic layers were washed with brine (3×150 ml)
  8. dry with materialdried over anhydrous sodium sulfate
  9. filtrationfiltered
  10. customThe solvent was removed under vacuum