참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethyl trifluoroacetate | HCID 9794 | — |
| 반응물 | Hexamethyldisilazane | HCID 13838 | — |
| 반응물 | 1-(4-(1H-Imidazol-1-yl)phenyl)ethanone | HCID 82316 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | Butane-1,3-dione, 4,4,4-trifluoro-1-(4-imidazol-1-ylphenyl)- | HCID 6426099 | — |
반응 단계
To a THF (5 mL) solution of 1,1,1,3,3,3-hexamethyldisilazane (0.178 g, 1.1 mmol) was added n-butyl lithum (1.6 M solution in hexane, 0.72 mL, 1.2 mmol) at 0° C. under nitrogen, and the mixture was stirred for 30 minutes, and cooled to −78° C. 4-(1-Imidazolyl)acetophenone (prepared according the method of M. A. Khan et. al., J. Chem. Soc. C., 1970, 85., 0.186 g, 1.0 mmol) was added to the mixture, and residue was stirred for 1 hour. Ethyl trifluoroacetate (0.17 g, 1.2 mmol) was added to the reaction mixture, the residure was warm to room temperature. The reaction mixture was poured into ice water and the whole was extracted with ethyl acetate (30 mL×2). The organic layer was washed with brine, dried over Na2SO4, and concentrated in vacuo. The resulting solid was washed with small amount of ethyl acetate to give the title compound (0.163 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06294558B1 |
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| 출처 데이터셋 | uspto-grants-2001_09 |
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| ORD ID | ord-dd99a2f70be241dfb12ab52cfb0b765d |
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| 출처 메모 | uspto-grants-2001_09 |
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