Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Tris(hydroxymethyl)aminomethane | HCID 6503 | — |
| Edukt | Dicyclohexylcarbodiimide | HCID 10868 | — |
| Edukt | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Edukt | 1-((Pyridin-4-yl)methyl)piperazine | HCID 808715 | — |
| Edukt | HCID 59420892 | HCID 59420892 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | HCID 59420891 | HCID 59420891 | — |
Reaktionsschritte
To a solution of 4-[3-(5-tert-butyl-2-methyl-2H-pyrazol-3-yl)-ureido]benzoic acid (0.08 g, 0.26 mmol) in a mixture of dichloromethane (4 mL) and DMF (0.20 mL) is added 1-(4-pyridinylmethyl)piperazine (0.046 g, 0.26 mmol), PS-DCC (0.41 g, 0.52 mmol) and HOBT (0.035 g, 0.26 mmol). The mixture is stirred overnight at 45° C. in a closed tube (orbital stirring). Then PS-Trisamine is added (0.52 mmol) and the mixture is stirred for 4 hr at room temperature, filtrated, and washed three times with dichloromethane. The solvents are evaporated under reduced pressure and the residue is purified by biotage column chromatography (eluent: ethyl acetate/methanol 10:1) to give 0.020 g (0.04 mmol), 16% as white solid. ES+(m/z)=476 [M+H].
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US07767674B2 |
|---|
| Quelldatensatz | uspto-grants-2010_08 |
|---|
| ORD ID | ord-813e2fcf51114c428f7ac57a1c0ba47b |
|---|
| Quellennotiz | uspto-grants-2010_08 |
|---|