Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Styrene | HCID 7501 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Tri-o-tolylphosphine | HCID 80271 | — |
| Reactant | HCID 86689064 | HCID 86689064 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67462533 | HCID 67462533 | — |
Reaction Steps
60 mg (128 μmol) 4-[6-(4-ethyl-6-oxo-1,4,5,6-tetrahydro-pyridazin-3-yl)-benzoxazol-2-yl]-phenyl trifluoro-methanesulphonate, 14.7 μl (128 μmol) styrene, 2.9 mg (13 μmol) palladium-(II)-acetate, 4.1 mg (13 μmol) tri-o-tolylphosphine, 72 μl (513 μmol) triethylamine and 2 ml acetonitrile are combined and stirred overnight at 80° C. Then a further 7.5 μl styrene, 2.9 mg palladium-(II)-acetate and 4 mg tri-o-tolyphosphine are added and the mixture is stirred for 5 days at 80° C. Then it is diluted with DCM and extracted successively with 10% sodium carbonate solution and sat. saline solution. The org. phase is evaporated down completely i.V. and the residue is purified through silica gel (eluant: DCM/methanol). The residue obtained is crystallised from cyclohexane/EA.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08772323B2 |
|---|
| Source dataset | uspto-grants-2014_07 |
|---|
| ORD ID | ord-7d6c52f3760b494c8c6deee24b294e4c |
|---|
| Source note | uspto-grants-2014_07 |
|---|
