化工社化工社 化学情報印刷レポート · 研究参考用
4-Nitroanthranilic acid → 2-(2,6-Difluoro-phenyl)-7-nitro-benzo[d][1,3]oxazin-4-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Nitroanthranilic acid | HCID 12076 | — |
| 反応物 | 2,6-Difluorobenzoyl chloride | HCID 87438 | — |
| 反応物 | 6-Acetamido-(2,6-difluoro-phenyl)-benzo[d][1,3]oxazin-4-one | HCID 9948813 | — |
| 反応物 | Toluene triethylamine | HCID 22504574 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-(2,6-Difluoro-phenyl)-7-nitro-benzo[d][1,3]oxazin-4-one | HCID 10447733 | — |
反応手順
4-Nitroanthranilic acid (0.6 g), 2,6-difluorobenzoyl chloride (0.93 mL) and triethyl amine/toluene (1/1) (18 mL) were reacted as described under (10). reaction time 2 days. Extraction between ethyl acetate (100 mL) and HCl (2N, 100 mL), followed by separation of the organic layer, drylng over MgSO4, filtering and evaporation gave a crude product which was dissolved in warm THF (20 mL) and precipitated with hexane twice to get the pure product 2-(2,6-difluoro-phenyl)-7-nitro-benzo[d][1,3]oxazin-4-one (0.417 g), mp. 187 C, MS m/e: 304 M+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06180625B2 |
| 出典データセット | uspto-grants-2001_01 |
| ORD ID | ord-ce17f9d856284bcd8eb7ba6a75536540 |
| 出典メモ | uspto-grants-2001_01 |