Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | 4-(Dimethylamino)benzoic acid | HCID 12092 | — |
| Edukt | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| Edukt | 1-Hydroxybenzotriazole hydrate | HCID 2796029 | — |
| Edukt | 2-Amino-4-(2-furyl)-5-(tetrahydropyran-4-ylcarbonyl)thiazole | HCID 86612468 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | HCID 23144247 | HCID 23144247 | 3% |
Reaktionsschritte
Compound 454 (125 mg, 0.450 mmol) was dissolved in DMF (2 mL), and 4-(dimethylamino)benzoic acid (296 mg, 1.80 mmol), EDC hydrochloride (344 mg, 1.80 mmol) and 1-hydroxybenzotriazole monohydrate (276 mg, 1.80 mmol) were added thereto, followed by stirring at 80° C. for 2 hours. Water (200 mL) was added to the reaction mixture, and the precipitated solid was collected by filtration. The resulting solid was purified through silica gel column chromatography (chloroform:methanol=9:1), followed by reslurrying with ethanol to afford the entitled Compound 465 (5.30 mg, 3%) as a pale brown solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US08889718B2 |
|---|
| Quelldatensatz | uspto-grants-2014_11 |
|---|
| ORD ID | ord-085f6fc3139b40f8a2820f687f555f21 |
|---|
| Quellennotiz | uspto-grants-2014_11 |
|---|
