반응 #1745

ord-9d8b4bad4cfc4f6f9993dde1eca90539

반응 방정식

OC1CCC(c2ccccc2)CC1
4-phenylcyclohexanol
CC(=O)OC(C)=O
acetanhydride
CC(=O)OC1CCC(c2ccccc2)CC1
O-acetyl-4-phenylcyclohexanol
수율 92.0%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONare added
  2. 2
    온도This is heated to 80° C. for 3 hours
  3. 3
    기타The crystalline product precipitated
  4. 4
    여과filtered
  5. 5
    workup.DISSOLUTIONdissolved in ether
  6. 6
    세척washed with sodium bicarbonate solution
  7. 7
    기타dried
  8. 8
    기타evaporated down in vacuo

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05726205uspto-grants-1998_03