HuagongsheHuagongshe Chemistry Print Report · For research reference only
Bromine → HCID 178517592, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Bromine | HCID 24408 | — |
| Reactant | 2(1H)-Pyridinone, 3-(trifluoromethyl)- | HCID 3678411 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 178517592 | HCID 178517592 | — |
Reaction Steps
A solution of 1.95 g (12 mmol) of 2-hydroxy-3-trifluoromethyl-pyridine and 0.8 mL of bromine in 10 mL of MeOH was stirred at rt for 20 h. The solution was concentrated and the residue partitioned between 100 mL of EtOAc and 25 mL of H2O. The layers were separated and the organic layer was washed with 25 mL of 5% Na2S2O3, 25 mL of sat'd NaCl, dried and concentrated. Chromatography on a Biotage 40 M cartridge using 3:1 hexanes/acetone as the eluant afforded 1.84 g of the title compound: ESI-MS (m/z) 242.1, 244.1; HPLC A: 2.22 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07605171B2 |
| Source dataset | uspto-grants-2009_10 |
| ORD ID | ord-a1198ba4a9bd40d5888d36d39826f2f7 |
| Source note | uspto-grants-2009_10 |