HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Diisopropylethylamine → HCID 67319417, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Diisopropylethylamine | HCID 81531 | — |
| Edukt | 2,6-Dimethylmorpholine, cis- | HCID 641500 | — |
| Edukt | 3,5-Difluoropyridine-2-carboxylic acid | HCID 2783262 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | HCID 67319417 | HCID 67319417 | 102,2% |
Reaktionsschritte
A solution of 3,5-difluoropicolinic acid (20.5 g, 128.86 mmol), cis-2,6-dimethylmorpholine (63.5 ml, 515.43 mmol) and DIEA (45.0 ml, 257.72 mmol) in THF (200 ml) was stirred at room temperature for 3 days. The mixture was diluted with EtOAc and extracted 3 times with aqueous Na2CO3. The aqueous layer was acidified with 1N HCl to bring pH to about 3 and was then saturated with NaCl before being extracted 10 times with EtOAc. The EtOAc layers were dried (MgSO4) and solvent was removed to give 33.5 g of product as a solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08658641B2 |
| Quelldatensatz | uspto-grants-2014_02 |
| ORD ID | ord-6144bb6c74bc472fad7fe332aca65051 |
| Quellennotiz | uspto-grants-2014_02 |