Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Edukt | 2-Amino-5-(trifluoromethyl)pyridine | HCID 735862 | — |
| Edukt | 3-Chloropyridine-2-carboxylic acid | HCID 824632 | — |
| Edukt | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| Lösungsmittel | Pyridine | HCID 1049 | — |
| Produkt | HCID 118113391 | HCID 118113391 | 34,2% |
Reaktionsschritte
A mixture of 0.81 g of 2-amino-5-trifluoromethylpyridine, 0.78 g of 3-chloropicolinic acid, 1.15 g of EDCI hydrochloride, 0.06 g of HOBt and 10 mL of pyridine was stirred at 60° C. for 2 hours. A saturated aqueous sodium bicarbonate solution was poured to the cooled reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and then concentrated under reduced pressure, and the resulting residue was applied to a silica gel column chromatography to obtain 0.51 g of 3-chloro-N-(5-trifluoromethylpyridin-2-yl)picolinamide.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US09185910B2 |
|---|
| Quelldatensatz | uspto-grants-2015_11 |
|---|
| ORD ID | ord-d031a8faadc349c4812ed05284448de7 |
|---|
| Quellennotiz | uspto-grants-2015_11 |
|---|
