HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → N-Pyridin-3-yl-4-[3-(3-thienyl)phenyl]piperazine-1-carboxamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Diisopropylethylamine | HCID 81531 | — |
| Edukt | 1-[3-(3-Thienyl)phenyl]piperazine | HCID 58985140 | — |
| Edukt | HCID 68575380 | HCID 68575380 | — |
| Lösungsmittel | Dimethyl Sulfoxide | HCID 679 | — |
| Produkt | N-Pyridin-3-yl-4-[3-(3-thienyl)phenyl]piperazine-1-carboxamide | HCID 16114127 | 37,4% |
Reaktionsschritte
A mixed solution of 2,2,2-trichloroethyl pyridin-3-ylcarbamate (303 mg, 1.13 mmol), 1-[3-(3-thienyl)phenyl]piperazine (250 mg, 1.02 mmol) and diisopropylethylamine (0.356 ml, 2.05 mmol) in dimethylsulfoxide (3.5 ml) was stirred at 70° C. for 3 days. Water was poured into the reaction solution, and extracted with ethyl acetate. The extract was washed with water, dried over anhydrous magnesium sulfate, and the solvent was distilled away under reduce pressure. The residue was purified by silica gel column chromatography (ethyl acetate), and recrystallized from a mixed solvent of hexane and tetrahydrofuran to give the titled compound 139 mg (37.3%) as solid product.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07812025B2 |
| Quelldatensatz | uspto-grants-2010_10 |
| ORD ID | ord-a0e2c83ccadb4bdf9c927cdbe862ecf0 |
| Quellennotiz | uspto-grants-2010_10 |