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Hydrochloric Acid → 6-Amino-2-methyl-3-nitrobenzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 6-Acetylamino-2-methyl-3-nitro-benzoic acid | HCID 15283171 | — |
| 溶媒 | Sodium Hydroxide | HCID 14798 | — |
| 生成物 | 6-Amino-2-methyl-3-nitrobenzoic acid | HCID 15283172 | 48% |
反応手順
A solution of 10.2 g (43 mmoles) of 5-nitro-6-methyl-2-acetylaminobenzoic acid in 100 mL of 2M NaOH was heated to reflux for two hours. The resultant red solution was allowed to cool to near room temperature, then transferred to a beaker sitting in an ice bath. The solution was slowly acidified with 2N HCl to a pH of approximately 4-5 when a voluminous yellow solid separated out. In all, approximately 110 mL of 2N HCl was added. The collected yellow solid was dried in a vacuum oven for 3 hours at 75 degrees. 4.0 g (48% yield) 5-nitro-6-methyl-2-aminobenzoic acid was obtained. NMR(DMSO-d6): 2.45 (s,3H), 3.35(bs,2H), 6.68(d,1H,J=9.0 Hz), 7.86(d,1H,J=9.0 Hz). MS(m/z): 196(M+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05428021 |
| 出典データセット | uspto-grants-1995_06 |
| ORD ID | ord-adeba882874f41c2af6f5027a5fb944a |
| 出典メモ | uspto-grants-1995_06 |