참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | N,O-Dimethylhydroxylamine | HCID 14232 | — |
| 반응물 | 2',4'-Dichloro-biphenyl-4-carbonyl chloride | HCID 57757250 | — |
| 용매 | Chloroform | HCID 6212 | — |
| 생성물 | 2',4'-Dichloro-biphenyl-4-carboxylic acid methoxy-methyl-amide | HCID 57757237 | — |
반응 단계
2′,4′-Dichloro-biphenyl-4-carbonyl chloride was dissolved in chloroform (10 mL) and added dropwise to a chilled solution of N,O-dimethyl hydroxylamine (2.5 g) and triethylamine (7 mL) in chloroform (40 mL). Following addition, the mixture was allowed to warm to room temperature and stirred for a further 30 minutes. The mixture was poured into water and the organic phase separated, washed with water, and dried. Evaporation gave an oil, which was purified by column chromatography (petrol/ethyl acetate) to give a pale yellow oil which slowly crystallised upon standing to give the title compound as a white solid. 13C NMR (CDCl3): δ 33.8, 61.2, 127.3, 128.2, 129.1, 129.9, 132.0, 133.2, 133.5, 134.2, 138.3, 140.5 and 169.5. 1H NMR (CDCl3): δ 3.39 (3H, s), 3.58 (3H, s), 7.26 (2H, m), 7.45 (2H, d, J=8.5 Hz), 7.54 (1H, s) and 8.08 (2H, d, J=8.5 Hz).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07560597B2 |
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| 출처 데이터셋 | uspto-grants-2009_07 |
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| ORD ID | ord-8c92664541dd458bbfc23d1637359098 |
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| 출처 메모 | uspto-grants-2009_07 |
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