Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | HCID 13007270 | HCID 13007270 | — |
| Reactant | HCID 178506053 | HCID 178506053 | — |
| Catalyst | HCID 178418397 | HCID 178418397 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 13007271 | HCID 13007271 | 81% |
Reaction Steps
A 1-liter reactor was charged with 31.2 g (0.10 mol) of 4-tert-butoxy-2,3-difluoro-1-iodobenzene and 100 ml of THF and heated at 60° C. To the reactor, 1.16 g (1 mmol) of tetrakis(triphenylphosphine)palladium(0) was added, then 300 ml of a THF solution of 1 M trifluorovinyl zinc iodide was added dropwise. After the completion of dropwise addition, the reaction solution was ripened for 30 minutes and poured into a saturated ammonium chloride aqueous solution. From the solution, a crude product was extracted with ethyl acetate in a conventional way. It was purified by silica gel chromatography, obtaining 21.5 g (yield 81%) the end product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US06333436B1 |
|---|
| Source dataset | uspto-grants-2001_12 |
|---|
| ORD ID | ord-cd0dec0ea75a4a7db0dfacee3bbdc6b8 |
|---|
| Source note | uspto-grants-2001_12 |
|---|