참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethanol | HCID 702 | — |
| 반응물 | Toluene | HCID 1140 | — |
| 반응물 | Di-tert-butyl peroxide | HCID 8033 | — |
| 반응물 | HCID 178418416 | HCID 178418416 | — |
| 촉매 | Cobalt(3+) acetylacetonate | HCID 407384 | — |
| 촉매 | 1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine) | HCID 636044 | — |
| 생성물 | Ethyl phenylacetate | HCID 7590 | 17.1% |
반응 단계
Toluene (1.38 g), ethanol (46 mg), di-tert-butyl peroxide (73 mg, 1 equivalent), cobalt acetylacetonate (1.3 mg, 1 mol %), and Xantphos (2.9 mg) were added into a reaction kettle, into which 10 atm carbon monoxide was introduced. The reaction was heated to 120° C., and stirred at this constant temperature for 16 h. After the reaction was completed, carbon monoxide was discharged, and 14 mg ethyl phenylacetate was obtained by column chromatography, in a yield of 17%. The ethyl phenylacetate obtained was dissolved in 1,4-dioxane. 6 N sodium hydroxide solution was added, and the reaction was heated to 60° C. After 2 h of reaction, the pH value was adjusted to 1 by adding 2 N hydrochloric acid. After removing the organic solvent under reduced pressure, 10 mg product phenylacetic acid was obtained by extraction with ethyl acetate, and the yield of hydrolysis was 93%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08921591B2 |
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| 출처 데이터셋 | uspto-grants-2014_12 |
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| ORD ID | ord-fc1cf4a8ca97498da9e93ee58aa98354 |
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| 출처 메모 | uspto-grants-2014_12 |
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