HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → 3-((2R,6S)-2,6-dimethylmorpholino)-5-fluoropicolinic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 2,6-Dimethylmorpholine, cis- | HCID 641500 | — |
| Reactant | 3,5-Difluoropyridine-2-carboxylic acid | HCID 2783262 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 3-((2R,6S)-2,6-dimethylmorpholino)-5-fluoropicolinic acid | HCID 67319417 | 102.2% |
Reaction Steps
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.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09040528B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-db710c14a54744bba97f591cd281d774 |
| Source note | uspto-grants-2015_05 |