참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Water | HCID 962 | — |
| 반응물 | Ethyl 6-(2',4'-dimethylphenyl)-6-cyano-3,3-dimethylhexanoate | HCID 13688117 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | 2-(2,4-Dimethylphenyl)-5,5-dimethylcyclohexane-1,3-dione | HCID 12556345 | 32% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04256657 |
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| 출처 데이터셋 | uspto-grants-1981_03 |
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| ORD ID | ord-cfb7a59c41894a1da68d7fdac50b7ebf |
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| 출처 메모 | uspto-grants-1981_03 |
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