化工社化工社 化学情報印刷レポート · 研究参考用
Acetic Acid → 3-Chloro-4,5-difluoroanthranilic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Tert-Butyl hypochlorite | HCID 521297 | — |
| 反応物 | 2-Amino-4,5-difluorobenzoic acid | HCID 735965 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 3-Chloro-4,5-difluoroanthranilic acid | HCID 21978924 | 100.8% |
反応手順
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+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07094780B1 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-cce603932cca4abba7de902112a6eb98 |
| 出典メモ | uspto-grants-2006_08 |