참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 2,4-Dichlorobenzoyl chloride | HCID 66645 | — |
| 반응물 | 1-(4-Bromo-2-hydroxyphenyl)ethan-1-one | HCID 10727403 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 2,4-Dichloro-benzoic acid 2-acetyl-5-bromo-phenyl ester | HCID 59788875 | 84% |
반응 단계
Triethylamine (14.6 mL, 104.6 mmol) was added to a solution of 1-(4-Bromo-2-hydroxy-phenyl)-ethanone (15.0 g, 96.8 mmol) dissolved in dichloromethane (200 mL). The resulting solution was cooled to 0° C. at which time 2,4-dichloro-benzoyl chloride, dissolved in 50 mL dichloromethane was added dropwise over 30 minutes. The resulting mixture was allowed to warm to ambient temperature and stir at this temperature for an additional 16 hours. After this time, the reaction mixture was concentrated via rotary evaporation and then dissolved in EtOAc and washed twice with water and once with a saturated NaHCO3 solution. The organic portion was dried (MgSO4), filtered and concentrated to give the desired product (22.7 g, 84%) which was used without further purification. 1H-NMR (DMSO) δ 8.18 (d, 1H), 7.96 (d, 1H), 7.82 (s, 1H), 7.64 (m, 3H), 2.53 (s, 3H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07420066B2 |
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| 출처 데이터셋 | uspto-grants-2008_09 |
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| ORD ID | ord-4fed5d305a384154ad38efb590cc7f20 |
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| 출처 메모 | uspto-grants-2008_09 |
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