HRID325939

反应详情

EQUATION

反应方程式

HRID 325939 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

A solution of 5.0 g of 3-methoxy-4-(2-ethoxy-1-oxapropyl)benzonitrile in 25 ml anhydrous THF was added dropwise to 119.5 ml 1 M lithium aluminum hydride in THF. The mixture was refluxed for four hours, cooled to 0° C., and the excess reagent was quenched with 5 N NaOH. The precipitated aluminum salts were removed by filtration and the THF evaporated. The residue was partitioned between 200 ml ether and 75 ml H2O. The remaining ether layer was washed with 75 ml of brine, dried (K2CO3), filtered, and evaporated to yield 3.63 g of 2-methoxy-4-aminomethyl-(2-ethoxy-1-oxapropyl)benzene.

WORKUP

后处理

  1. temperatureThe mixture was refluxed for four hours
  2. customthe excess reagent was quenched with 5 N NaOH
  3. customThe precipitated aluminum salts were removed by filtration
  4. customthe THF evaporated
  5. customThe residue was partitioned between 200 ml ether and 75 ml H2O
  6. washThe remaining ether layer was washed with 75 ml of brine
  7. dry with materialdried (K2CO3)
  8. filtrationfiltered
  9. customevaporated