참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 1,4-Dithiane-2,5-diol | HCID 98330 | — |
| 반응물 | 3-(4-Methylphenyl)-3-oxopropanenitrile | HCID 522513 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | 3-(4-Methylbenzoyl)thiophen-2-amine | HCID 859626 | 130.2% |
반응 단계
To a suspension of 4-methylbenzoylacetonitrile (0.325 g; 2.042 mmol) and p-dithiane-2,5-diol (0.155 g; 1.018 mmol) in ethanol (4.3 mL) cooled at 0° C. was added triethylamine (0.283 mL; 2.042 mmol). After 10 min at room temperature, the reaction mixture was heated under reflux for 2 h. After cooling to room temperature, the reaction mixture was partitioned between ethyl acetate and water. The organic phase was washed with brine, dried over sodium sulphatesulphate, filtered and concentrated under reduced pressure. The residue was purified by flash chromatography on silica gel using a gradient of ethyl acetate (10-25%) in heptane to afford the title compound (0.288 g; 65%) as a yellow solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08785638B2 |
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| 출처 데이터셋 | uspto-grants-2014_07 |
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| ORD ID | ord-d5fc8a55d4d84a2daa06bb9f151e5ed1 |
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| 출처 메모 | uspto-grants-2014_07 |
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