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Hydrochloric Acid → 6-Acetamido-(2,6-difluoro-phenyl)-benzo[d][1,3]oxazin-4-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2,6-Difluorobenzoyl chloride | HCID 87438 | — |
| 反応物 | Benzoic acid, 5-(acetylamino)-2-amino- | HCID 170890 | — |
| 反応物 | 2-(2,6-Difluoro-phenyl)-6-nitro-benzo[d][1,3]oxazin-4-one | HCID 21262464 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | Toluene triethylamine | HCID 22504574 | — |
| 生成物 | 6-Acetamido-(2,6-difluoro-phenyl)-benzo[d][1,3]oxazin-4-one | HCID 9948813 | 94% |
反応手順
5-Acetamidoanthranilic acid (0.64g) and 2,6-difluorobenzoyl chloride (1.3 g) were reacted in triethyl amine/toluene (1/1) (20 mL) like described for compound (9), reaction time 1 h. Ethyl acetate (50 mL) and HCl-solution (1 mL 4N in 50 mL water) were added resulting in the formation of a precipitate.The mixture was filtered and the residue dissolved in THF followed by evaporation to dryness, subsequent dissolution in hot dioxane followed by precipitation with hexane resulted in colourless crystals of 6-acetamido-(2,6-difluoro-phenyl)-benzo[d][1,3]oxazin-4-one (0.98 g), mp.246 C, MS m/e.: 316 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-3e485fe52fe24eaab6bc8b1cb4ca842a |
| 出典メモ | uspto-grants-2001_01 |