HuagongsheHuagongshe Chemistry Print Report · For research reference only
Nitrogen → 2-Fluoro-3-trifluoromethyl-4-vinylaniline
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Nitrogen | HCID 947 | — |
| Reactant | 4-Bromo-2-fluoro-3-(trifluoromethyl)aniline | HCID 53669714 | — |
| Reactant | Tributylvinyltin chloride | HCID 86633508 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 2-Fluoro-3-trifluoromethyl-4-vinylaniline | HCID 68821544 | — |
Reaction Conditions
| Temperature | 120 °C |
|---|
Reaction Steps
4-Bromo-2-fluoro-3-trifluoromethylaniline described above (5.0 g, 19.4 mmol) and tributylvinyltin chloride (7.1 g, 20.4 mmol) are added to anhydrous DMF (100 mL). The solution is degassed with N2, palladium tetrakistriphenylphosphine (1.5 g, 1.3 mmol) is added, and the reaction is heated at 120° C. for 18 hours. After cooling, the reaction mixture is partitioned between Et2O and saturated aqueous NaCl. The separated ether layer is washed with fresh saturated aqueous NaCl (2×), dried with Na2SO4, and concentrated under reduced pressure. The residue is purified by flash chromatography eluting with 5, then 10, then 20% EtOAc in hexanes to give the desired product, 2-fluoro-3-trifluoromethyl-4-vinylaniline.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08362294B2 |
| Source dataset | uspto-grants-2013_01 |
| ORD ID | ord-b23fb36a00544ed0bba69c20bf831d51 |
| Source note | uspto-grants-2013_01 |