Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Acetic Acid → 3-Chloro-4,5-difluoroanthranilic acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | Tert-Butyl hypochlorite | HCID 521297 | — |
| 반응물 | 2-Amino-4,5-difluorobenzoic acid | HCID 735965 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 3-Chloro-4,5-difluoroanthranilic acid | HCID 21978924 | 100.8% |
반응 단계
To a solution of 4,5-difluoroanthranilic acid (2.45 g, 14.2 mmol) in dichloromethane (25 mL) is added acetic acid (10 mL) and hypochlorous acid tert-butyl ester (1.75 mL, 15.6 mmol). After 2 hours, the reaction mixture is diluted with ethyl acetate and washed with water and brine. The organic layer is dried over MgSO4, filtered, and concentrated. The resulting residue is purified via flash column chromatography (5% isopropyl alcohol/1% formic acid/94% dichloromethane) to afford 3-chloro-4,5-difluoroanthranilic acid as an oil (2.97 g). MS CI: m/z 206 (M+).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07094780B1 |
| 출처 데이터셋 | uspto-grants-2006_08 |
| ORD ID | ord-cce603932cca4abba7de902112a6eb98 |
| 출처 메모 | uspto-grants-2006_08 |