HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 86728475, compound → HCID 86728476, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 86728475 | HCID 86728475 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Hydrogen Bromide | HCID 260 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 86728476 | HCID 86728476 | 72% |
Reaction Conditions
| Temperature | 100 °C |
|---|
Reaction Steps
2-fluoro-N-(2-methoxy-4-pyridyl)-4-(1,1,2,2,2-pentafluoroethyl)benzamide (200 mg, 0.55 mmol) in HBr in acetic acid (1.3 mL of 33% w/v, 5.49 mmol) was stirred at 100° C. for 2 hours, at this time 1 ml of HBr in acetic acid (33% w/v) was added and the mixture was stirred at 100° C. for 4 hours, then cooled to room temperature. The reaction mixture was diluted with water and a precipitate formed. The precipitate was filtered off, washed with water (2×), cold methyl-tert-butyl ether and dried under vacuum to give 2-fluoro-N-(2-oxo-1H-pyridin-4-yl)-4-(1,1,2,2,2-pentafluoroethyl)benzamide (138 mg, 72%) as a light grey solid. ESI-MS m/z calc. 350.05, found 351.3 (M+1)+; Retention time: 1.3 minutes (3 minutes run).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09163042B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-c889af3336ec4eef9a60af44c743b268 |
| Source note | uspto-grants-2015_10 |