HRID1414270

反应详情

EQUATION

反应方程式

HRID 1414270 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a suspension of 20 parts of lithium aluminum hydride in 444 parts of tetrahydrofuran and 177 parts of ethyl ether is added portionwise, over a 1 hour period, a warm solution of 56 parts of 3-benzyloxy-4-methoxy-β-nitrostyrene in 267 parts of tetrahydrofuran. The reaction mixture is refluxed for an additional 2 hours, then is cooled in ice and decomposed by adding 40 parts of water in 71 parts of tetrahydrofuran, followed by 40 parts by volume of a 25% by weight aqueous sodium hydroxide solution, followed by 40 parts of water. The salts are removed by filtration and the filtrate is dried over anhydrous calcium sulfate and stripped of solvent under reduced pressure to afford, as an oil, 3-benzyloxy-4-methoxyphenethylamine.

WORKUP

后处理

  1. additionis added portionwise, over a 1 hour period
  2. temperatureThe reaction mixture is refluxed for an additional 2 hours
  3. temperatureis cooled in ice
  4. customThe salts are removed by filtration
  5. dry with materialthe filtrate is dried over anhydrous calcium sulfate