Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → (E)-4-bromo-3-(2-chloro-phenoxy)-but-2-enoic acid ethyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | N-bromobutanimide | HCID 67184 | — |
| 반응물 | (E)-3-(2-chloro-phenoxy)-but-2-enoic acid ethyl ester | HCID 66894719 | — |
| 촉매 | 2,2'-Azobis(2,4-dimethylvaleronitrile) | HCID 91537 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | (E)-4-bromo-3-(2-chloro-phenoxy)-but-2-enoic acid ethyl ester | HCID 66895331 | 113% |
반응 단계
To a solution of (E)-3-(2-chloro-phenoxy)-but-2-enoic acid ethyl ester (1880 g, 7.82 mol) in dichloromethane (18.6 L) was added N-bromosuccinimide (1490 g, 8.29 mol) and 2,2′-azobis(2,4-dimethylvaleronitrile) (47 g, 0.188 mol) and the resulting solution heated to reflux for 23 h. The light yellow solution was cooled to room temperature and transferred to an extractor before water (19 L) was added. The biphasic mixture was stirred at room temperature for 1 h. The mixture was separated and the organic phase washed with a 20% sodium chloride solution (19 L). The solution was evaporated to give (E)-4-bromo-3-(2-chloro-phenoxy)-but-2-enoic acid ethyl ester (87.8% pure by HPLC, 2824 g, 99%) as a red oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07741327B2 |
| 출처 데이터셋 | uspto-grants-2010_06 |
| ORD ID | ord-1cf7c89fa3a8465e90568a968c046442 |
| 출처 메모 | uspto-grants-2010_06 |