HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 57469060, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 60209477 | HCID 60209477 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 57469060 | HCID 57469060 | 46% |
Reaction Steps
To a cooled and stirred solution of 5-{1-[4-(3,4-difluoro-phenyl)-6-trifluoromethyl-pyrimidin-2-yl]-1H-imidazol-4-yl}-thiophene-2-sulfonic acid tert-butyl amide (0.24 g) in dichloromethane (4 ml) was added TFA (4 ml) and the reaction mixture was allowed to stir at room temperature for 15 h. The mixture was evaporated to dryness, poured into 2N NaHCO3 solution (25 ml) and extracted ethyl acetate (3×50 ml). The combined organic layers were washed with brine (50 ml), dried (MgSO4) and evaporated. Further purification by flash chromatography on silica gel (MeOH/dichloromethane) and crystallization (dichloromethane/heptane) yielded the title compound as a light yellow solid (0.077 g, 46%). MS (ISP) 487.9 [(M+H)+]; mp 228° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07642264B2 |
| Source dataset | uspto-grants-2010_01 |
| ORD ID | ord-4648840b3856482ab35e1a9f6cb4f6c8 |
| Source note | uspto-grants-2010_01 |