Acetic Anhydride → (4-Phenylcyclohexyl) acetate

HRID 1737930

반응식

HRID 1737930 반응식
[C:1]1([CH:7]2[CH2:12][CH2:11][CH:10]([OH:13])[CH2:9][CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:14][C:15](OC(C)=O)=[O:16]>CN(C)C1C=CN=CC=1.C(N(CC)CC)C>[C:15]([O:13][CH:10]1[CH2:9][CH2:8][CH:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[CH2:12][CH2:11]1)(=[O:16])[CH3:14]

참가 물질

5

반응물 2

HCID 7918Acetic AnhydrideHCID 794974-Phenylcyclohexanol

생성물 1

HCID 226557(4-Phenylcyclohexyl) acetate수율 92%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 8471Triethylamine용매

실험 절차

To a mixture of 20.3 g (0.115 mol) of 4-phenylcyclohexanol, 14.2 ml (O.1S 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. Melting point: 43-45° C.

후처리

  1. additionare added
  2. temperatureThis is heated to 80° C. for 3 hours
  3. customThe crystalline product precipitated
  4. filtrationfiltered
  5. dissolutiondissolved in ether
  6. washwashed with sodium bicarbonate solution
  7. customdried
  8. customevaporated down in vacuo

출처 및 근거

ORD 기록
ord-40645d504a3548508b2f0fa33711be8b
출처 데이터셋
uspto-grants-1999_10
특허 번호
US05962507

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