HRID132743

反应详情

EQUATION

反应方程式

HRID 132743 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

While cooled by an ice-bath and stirred intensely, 0.0 mol 1,5-diphenyl-1,5-pentandione was added dropwise slowly to a mixture of 3 g LiAlH4 and 100 ml anhydrous tetrahydrofuran. The mixture was heated refluxing for 5 hours, then cooled. Excess LiAlH4 was decomposed with water. After mixing completely the reaction mixture with ethyl acetate, the mixture was filtered, and the filtrate was dried over anhydrous sodium sulfate. The solvent was removed. Column chromatography gave 1,5-diphenyl-1,5-pentanediol as a white solid, and the yield was 85%. mp: 64-67° C. IR spectrum had a strong —OH absorption peak at 3400 cm−1, and had no —CO— absorption peak at about 1700 cm−1. This demonstrated that the reduction reaction was carried out completely.

WORKUP

后处理

  1. temperatureWhile cooled by an ice-bath
  2. temperatureThe mixture was heated
  3. temperaturerefluxing for 5 hours
  4. temperaturecooled
  5. filtrationthe mixture was filtered
  6. dry with materialthe filtrate was dried over anhydrous sodium sulfate
  7. customThe solvent was removed