HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Nitrobenzoic Acid → (4-Methylpiperazin-1-yl)(4-nitrophenyl)methanone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Nitrobenzoic Acid | HCID 6108 | — |
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| Solvent | Water | HCID 962 | — |
| Product | (4-Methylpiperazin-1-yl)(4-nitrophenyl)methanone | HCID 716396 | 95% |
Reaction Steps
To a solution of 4-nitro-benzoic acid (10 g, 0.0598 mol) in DMF (300 mL) 1-methyl-piperazine (7.19 g, 0.0718 mol), HOBt (10.5 g, 0.0777 mol), EDC.HCl (17.12 g, 0.0897 mol) and TEA (12.1 g, 0.1196 mol) were added. The reaction mixture was stirred at room temperature for 12 h. The reaction mixture was diluted with water and extracted with ethyl acetate (3×200 mL). The organic layer was washed with water, brine and dried over sodium sulfate. The solvent was evaporated under reduced pressure to afford the title compound [14 g, 95%]; LC-MS (ESI): Calculated mass: 249.1; Observed mass: 250.0 [M+H]+ (RT: 0.10 min).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09115092B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-8d48607d66c047a9bbdb2b1f6065fe83 |
| Source note | uspto-grants-2015_08 |