HRID1351756

反应详情

EQUATION

反应方程式

HRID 1351756 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 18 g (0.075 mol) of 2-ethoxycarbonylaminobiphenyl in 100 ml of THF is added dropwise to a suspension of 14.2 g (0.373 mol) of lithium aluminum hydride in 300 ml of THF. The mixture is stirred for another 1 hour and then refluxed for 3 hours. Subsequently, while cooling in ice, 28 ml of water are firstly added dropwise and 18 ml of 15% strength aqueous sodium hydroxide are then added. After the precipitate has been separated off, it is washed a number of times with ether. The combined filtrates are dried over sodium sulfate, and the reddish liquid obtained after evaporation of the solvent is fractionated at 0.01 mbar. Bp.: 65–67° C. Yield: 10.64 g=77%.

WORKUP

后处理

  1. temperaturerefluxed for 3 hours
  2. temperatureSubsequently, while cooling in ice
  3. customAfter the precipitate has been separated off
  4. washit is washed a number of times with ether
  5. dry with materialThe combined filtrates are dried over sodium sulfate
  6. customthe reddish liquid obtained
  7. customafter evaporation of the solvent