反应 #1745

ord-9d8b4bad4cfc4f6f9993dde1eca90539

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONare added
  2. 2
    温度This is heated to 80° C. for 3 hours
  3. 3
    其他The crystalline product precipitated
  4. 4
    过滤filtered
  5. 5
    workup.DISSOLUTIONdissolved in ether
  6. 6
    洗涤washed with sodium bicarbonate solution
  7. 7
    其他dried
  8. 8
    其他evaporated down in vacuo

实验过程

To a mixture of 20.3 g (0.115 mol) of 4-phenylcyclohexanol, 14.2 ml (0.15 mol) of acetanhydride and 29 ml of triethylamine are added, with stirring and at ambient temperature, 2.3 g (0.02 mol) of 4-dimethylaminopyridine, a clear solution being produced in an exothermic reaction. This is heated to 80° C. for 3 hours and the reaction mixture is then poured into ice water. The crystalline product precipitated is suction filtered, dissolved in ether, washed with sodium bicarbonate solution, dried and evaporated down in vacuo. 23 g (92% of theory) of O-acetyl-4-phenylcyclohexanol are obtained. The product is obtained initially as an oil but crystallises when left to stand.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05726205uspto-grants-1998_03