참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1-Phenyl-1-propanone | HCID 7148 | — |
| 반응물 | Chlorobenzene | HCID 7964 | — |
| 반응물 | Tetrahydrofuran | HCID 8028 | — |
| 반응물 | Sodium t-butoxide | HCID 23676156 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 촉매 | Tri-tert-butylphosphonium Tetraphenylborate | HCID 23136663 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 1,2-Diphenylpropan-1-one | HCID 238518 | 77.4% |
반응 단계
A 30-ml four-necked flask was equipped with a stirrer, a thermometer and a reflux condenser. 0.022 g (0.1 mmol) of palladium (II) acetate, 0.721 g (7.5 mmol) of sodium-tert-butoxide and 5 ml of tetrahydrofuran were weighed in the flask, followed by stirring. Further, 0.052 g (0.1 mmol) of tri-tert-butylphosphonium tetraphenylborate obtained in Example A-1 was weighed in air and added into the flask. The flask was purged with argon, followed by stirring at 22° C. for 30 minutes. 0.563 g (5 mmol) of chlorobenzene was added, followed by stirring at 22° C. for 30 minutes. 0.738 g (5.5 mmol) of propiophenone was added, followed by stirring at 70° C. for 6 hours. After the completion of the reaction, 2.5 ml of water was added, followed by separation. The organic phase was purified by column chromatography to afford 0.814 g of 1,2-diphenyl-1-propanone (yield: 77 mol % based on chlorobenzene). The identification of the product was made by mass spectroscopy, 1H-NMR and 13C-NMR.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07728176B2 |
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| 출처 데이터셋 | uspto-grants-2010_06 |
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| ORD ID | ord-63185a4f26d44eaa9e2876f42025d9bf |
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| 출처 메모 | uspto-grants-2010_06 |
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