Acetic Acid → 2-(2,4-Dimethylphenyl)-5,5-dimethylcyclohexane-1,3-dione

HRID 127543

반응식

HRID 127543 반응식
[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][C:3]=1[CH:9](C#N)[CH2:10][CH2:11][C:12]([CH3:20])([CH3:19])[CH2:13][C:14]([O:16]CC)=O.Cl.C(O)(=[O:26])C.O>C(OCC)C>[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][C:3]=1[CH:9]1[C:10](=[O:26])[CH2:11][C:12]([CH3:19])([CH3:20])[CH2:13][C:14]1=[O:16]

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 313Hydrochloric Acid2회HCID 962Water2회HCID 13688117Ethyl 6-(2',4'-dimethylphenyl)-6-cyano-3,3-dimethylhexanoate

생성물 1

HCID 125563452-(2,4-Dimethylphenyl)-5,5-dimethylcyclohexane-1,3-dione수율 32%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

A one-neck round bottom flask was charged with 52.50 g (0.17 mol) of ethyl 6-(2',4'-dimethylphenyl)-6-cyano-3,3-dimethylhexanoate, 250 ml of concentrated hydrochloric acid, 250 ml of glacial acetic acid, and 100 ml of water. The reaction mixture was stirred and refluxed for 48 hours. After 12 hours and 24 hrs. of refluxing, an additional 100 ml of conc. HCl and 100 ml glacial HOAC were added. After 48 hours, the mixture was stripped to dryness under reduced pressure. To the residue were added 150 ml of water and 150 ml of ethyl ether, and the mixture shaken vigorously. A white, crystalline precipitate formed, and this was removed by suction filtration to give 13.20 g (32%) of 2-(2',4'-Dimethylphenyl)-5,5-dimethyl-1,3-cyclohexanedione as a white, crystalline solid, m.p. 167°-168.5° C.

후처리

  1. temperaturerefluxed for 48 hours
  2. custom24 hrs
  3. temperatureof refluxing
  4. waitAfter 48 hours
  5. stirringthe mixture shaken vigorously
  6. customA white, crystalline precipitate formed
  7. customthis was removed by suction filtration

출처 및 근거

ORD 기록
ord-11a8000962fa49ddbf0bff24f0ab9a5a
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04256659

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