HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → (S)-2,2-Difluoro-2-(1-hydroxy-3,3,5,5-tetramethylcyclohexyl)-1-(2-(5-((pyridin-3-yloxy)methyl)isoxazol-3-yl)pyrrolidin-1-yl)ethanone hydrochloride monohydrate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Setafrastat | HCID 73672050 | — |
| Solvent | Pentane | HCID 8003 | — |
| Product | (S)-2,2-Difluoro-2-(1-hydroxy-3,3,5,5-tetramethylcyclohexyl)-1-(2-(5-((pyridin-3-yloxy)methyl)isoxazol-3-yl)pyrrolidin-1-yl)ethanone hydrochloride monohydrate | HCID 86706783 | — |
Reaction Steps
To an AcOEt (50 ml) solution of Compound 40 (2.24 g) obtained in Example 2, HCl (50 ml, 4.0 N in AcOEt) was added and the mixture was stirred at room temperature for 15 hours, and after adding pentane (140 ml), the mixture was stirred for 8 days. The residue obtained by concentrating the reaction mixture was recrystallized (MeOH/Et2O) to give the titled compound (2.23 g, colorless powder.)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09181229B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-63cb76eccbd6493b9ed8108ffee04d80 |
| Source note | uspto-grants-2015_11 |