HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Diisopropylethylamine → HCID 57378953, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Diisopropylethylamine | HCID 81531 | — |
| Edukt | Propylphosphoric anhydride | HCID 16167369 | — |
| Edukt | 4-(Methoxycarbonyl)-1-methyl-1H-pyrazole-5-carboxylic acid | HCID 45923681 | — |
| Edukt | 2-Phenyl-[1,2,4]triazolo[1,5-a]pyridin-7-ylamine | HCID 67774145 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Lösungsmittel | Sodium Bicarbonate | HCID 516892 | — |
| Produkt | HCID 57378953 | HCID 57378953 | 94,5% |
Reaktionsschritte
A solution of 2-phenyl-[1,2,4]triazolo[1,5-a]pyridin-7-ylamine (1.534 g, 7.3 mmol), 4-(methoxycarbonyl)-1-methyl-1H-pyrazole-5-carboxylic acid (1.61 g, 8.76 mmol), propylphosphonic anhydride (50% in ethyl acetate, 10.7 ml, 18.2 mmol) and diisopropylethylamine (5.1 ml, 29.2 mmol) in tetrahydrofurane (54 ml) is stirred at 70° C. for 1.25 hr giving a white suspension. The cooled suspension is poured in sat. aqueous sodium bicarbonate solution (200 ml), stirred at room temperature for 15 min and the solid is collected by filtration, washed with water and dried affording methyl 1-methyl-5-(2-phenyl-[1,2,4]triazolo[1,5-a]pyridin-7-ylcarbamoyl)-1H-pyrazole-4-carboxylate (2.596 g, 94.5%) as a white solid. mp.: 243-7° C. MS: m/z=377.2 (M+H+).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08349824B2 |
| Quelldatensatz | uspto-grants-2013_01 |
| ORD ID | ord-855055d4ec904c1a96d094e383d2d916 |
| Quellennotiz | uspto-grants-2013_01 |