참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 3-Dimethylaminobenzoyl chloride | HCID 7010342 | — |
| 반응물 | Ethyl 4-(4-aminophenyl)butanoate | HCID 10013251 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 4-[4-(3-Dimethylamino-benzoylamino)-phenyl]-butyric acid ethyl ester | HCID 67045331 | 97.5% |
반응 단계
A solution of 3-dimethylaminobenzoyl chloride (0.19 g, 1.01 mmol) in THF (6 ml) was added dropwise to a solution of 4-(4-aminophenyl)butyric acid ethyl ester (0.26 g, 1.24 mmol) and triethylamine (0.31 g, 3.11 mmol) in THF (8 ml) under ice cooling. The reaction solution was stirred at room temperature for 8 hours, then added with water, and extracted with ethyl acetate. The ethyl acetate layer was washed with saturated aqueous ammonium chloride and saturated brine, then dried over sodium sulfate, filtered, and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=15:1) to obtain 4-[4-(3-dimethylamino-benzoylamino)-phenyl]-butyric acid ethyl ester as a brown oily substance (0.36 g, yield: 97.5%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08722723B2 |
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| 출처 데이터셋 | uspto-grants-2014_05 |
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| ORD ID | ord-537ee15699e143968a5b63286d5a401a |
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| 출처 메모 | uspto-grants-2014_05 |
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