HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridinium, 1-fluoro-, 1,1,1-trifluoromethanesulfonate (1:1) → 3-fluoro-2-methyl-4-(trifluoromethyl)-1H-indole-5-carbonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridinium, 1-fluoro-, 1,1,1-trifluoromethanesulfonate (1:1) | HCID 2724576 | — |
| Reactant | 2-methyl-4-(trifluoromethyl)-1H-indole-5-carbonitrile | HCID 53309346 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 3-fluoro-2-methyl-4-(trifluoromethyl)-1H-indole-5-carbonitrile | HCID 57800310 | 22.1% |
Reaction Steps
To a solution of 2-methyl-4-(trifluoromethyl)-1H-indole-5-carbonitrile (0.063 g, 0.28 mmol) in CH2Cl2 (4 mL) was added 1-fluoropyridinium triflate (0.104 g, 0.42 mmol) and stirred at rt for 3 days. The mixture was partitioned between EtOAc and 0.1N HCl. The organic phase was washed with 0.1N HCl and sat'd brine, dried (Na2SO4), and concentrated in vacuo. The residue was purified by flash chromatography (10-50% EtOAc-hexanes gradient) to afford the title compound as a white solid (0.015 g, 22% yield, 94% purity): MS (ES) m/z 243 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08026262B2 |
| Source dataset | uspto-grants-2011_09 |
| ORD ID | ord-a8864ad720984882b6b423efc4a26f5d |
| Source note | uspto-grants-2011_09 |