HRID1451512

反应详情

EQUATION

反应方程式

HRID 1451512 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 3-benzylbenzoic acid (15 g, 70 mmol) in THF (100 ml) a solution of lithium aluminiumhydride in THF (80 ml, 80 mmol, 1M) was added dropwise. When addition was complete the mixture was stirred for 30 minutes at ambient temperature and then heated at reflux for 40 minutes. The reaction mixture was allowed to cool and water (3 ml), diethyl ether (100 ml), 4N sodium hydroxide (6 ml) and water (12 ml) were added successively. The mixture was stirred for 30 minutes, filtered and the solvent evaporated in vacuo. The residue was dissolved in toluene (200 ml) and dried (MgSO4) overnight. The solvent was evaporated in vacuo to give 11.9 g of crude 3-benzylbenzylalcohol as an oil.

WORKUP

后处理

  1. additionwas added dropwise
  2. additionWhen addition
  3. temperatureheated
  4. temperatureat reflux for 40 minutes
  5. temperatureto cool
  6. stirringThe mixture was stirred for 30 minutes
  7. filtrationfiltered
  8. customthe solvent evaporated in vacuo
  9. dissolutionThe residue was dissolved in toluene (200 ml)
  10. dry with materialdried (MgSO4) overnight
  11. customThe solvent was evaporated in vacuo