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Hydrochloric Acid → 2-Methyl-5-nitro-4-(4-o-tolyl-piperazin-1-yl)-benzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-(o-Tolyl)piperazine dihydrochloride | HCID 91964 | — |
| 反応物 | 4-Fluoro-2-methyl-5-nitrobenzoic acid | HCID 22313101 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Methyl-5-nitro-4-(4-o-tolyl-piperazin-1-yl)-benzoic acid | HCID 89690648 | — |
反応手順
To a stirred solution of 4-fluoro-2-methyl-5-nitro-benzoic acid (5.0 g, 25.10 mmol) in anhydrous DMF (100 mL), potassium carbonate (10.4 g, 75.3 mmol) was added under N2 atmosphere followed by 1-o-tolyl-piperazine 2 HCl (8.13 g, 32.6 mmol). The reaction mixture was allowed to stir at room temperature overnight. The progress of the reaction was checked by TLC, upon completion of the reaction, solvent was removed in vacuo. The residue obtained was acidified with conc. HCl (≈pH=2-3). Yellow solid obtained was filtered and washed with water (3×75 mL), diethyl ether and dried under vacuo to obtain the pure product 2-methyl-5-nitro-4-(4-o-tolyl-piperazin-1-yl)-benzoic acid. Yield (6.5 g, 73%; and yellow solid).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09409897B2 |
| 出典データセット | uspto-grants-2016_08 |
| ORD ID | ord-ed984582d8f44b28aed168943abd906e |
| 出典メモ | uspto-grants-2016_08 |