HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → 2-Methyl-5-nitro-4-(4-o-tolyl-piperazin-1-yl)-benzoic acid
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 1-(o-Tolyl)piperazine dihydrochloride | HCID 91964 | — |
| Edukt | 4-Fluoro-2-methyl-5-nitrobenzoic acid | HCID 22313101 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 2-Methyl-5-nitro-4-(4-o-tolyl-piperazin-1-yl)-benzoic acid | HCID 89690648 | — |
Reaktionsschritte
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).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09409897B2 |
| Quelldatensatz | uspto-grants-2016_08 |
| ORD ID | ord-ed984582d8f44b28aed168943abd906e |
| Quellennotiz | uspto-grants-2016_08 |