Acetic Anhydride → (4-Phenylcyclohexyl) acetate

HRID 1649

反応式

HRID 1649 の反応式
[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]

参加物

5

反応物 2

HCID 7918Acetic AnhydrideHCID 794974-Phenylcyclohexanol

生成物 1

HCID 226557(4-Phenylcyclohexyl) acetate収率 92%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 8471Triethylamine溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9d8b4bad4cfc4f6f9993dde1eca90539
出典データセット
uspto-grants-1998_03
特許番号
US05726205

関連ノート

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