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Nitric Acid → 4-Acetamido-2-hydroxy-5-nitrobenzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | 4-Acetamidosalicylic acid | HCID 65509 | — |
| 溶媒 | Trifluoroacetic acid | HCID 6422 | — |
| 生成物 | 4-Acetamido-2-hydroxy-5-nitrobenzoic acid | HCID 67287438 | 28% |
反応手順
Nitric acid (fuming) (23.8 g, 378 mmol, 1.20 equiv) was added in portions under 50° C. to a mixture of 4-acetamido-2-hydroxybenzoic acid (61.4 g, 315 mmol, 1.00 equiv) and TFA (700 mL) in a 2-L round-bottom flask. The resulting solution was allowed to react, with stirring, for 3 hr at room temperature before being concentrated under vacuum. The residue was dissolved in 800 mL of acetone, stirred for 15 min. at reflux, then cooled. The solids were collected by filtration, giving 21.1 g (28%) of 4-acetamido-2-hydroxy-5-nitrobenzoic acid as an orange solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09370522B2 |
| 出典データセット | uspto-grants-2016_06 |
| ORD ID | ord-6eff936efc6a4aeb84ebc961e2d0f6fc |
| 出典メモ | uspto-grants-2016_06 |