HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ammonium Chloride → 5-tert-butyl-1-(2'-chloro-1,1'-biphenyl-3-yl)-1H-pyrazole-3-carboxamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ammonium Chloride | HCID 25517 | — |
| Edukt | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Edukt | N,N-Diethyl-2-propanamine | HCID 521913 | — |
| Edukt | 5-tert-butyl-1-(2'-chloro-1,1'-biphenyl-3-yl)-1H-pyrazole-3-carboxylic acid | HCID 11279690 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 5-tert-butyl-1-(2'-chloro-1,1'-biphenyl-3-yl)-1H-pyrazole-3-carboxamide | HCID 11382645 | 103,1% |
Reaktionsschritte
To a solution of the carboxylic acid (0.062 g, 0.17 mmol) in DMF (1 ml) were added pyBOP (0.138 g, 0.26 mmol), HOBT (0.035 g, 0.2 mmol), diethylisopropylamine (0.147 ml, 0.87 mmol) and ammonium chloride (0.056 g, 1.05 mmol). The reaction mixture was stirred at room temperature for 16 hours, then cooled and partitioned between ethylacetate and water. The organic phase was washed with brine, dried over sodium sulfate, filtered and concentrated. Purification of the crude product by silica-gel chromatography (3:2 hexanes/ethylacetate) yielded the product (0.062 g, 64%) as a solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07589116B2 |
| Quelldatensatz | uspto-grants-2009_09 |
| ORD ID | ord-be7ac90ca35c4ec0ad5442cbff5b3004 |
| Quellennotiz | uspto-grants-2009_09 |