HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 22714700, compound → HCID 22714702, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 22714700 | HCID 22714700 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 22714702 | HCID 22714702 | — |
Reaction Steps
A solution composed of 55.94 g of 6-trifluoroacetyl-1-benzocyclobutanecarbonitrile in 600 ml of pyridine is purged with nitrogen for 15 minutes; 30.5 ml of triethylamine, 117.44 ml of butyl vinyl ether, 2.25 g of 1,3-bis-(diphenylphosphino)propane and 1.02 g of palladium acetate are added and the reaction mixture is heated at reflux for 2 hours. 400 ml of 1N hydrochloric acid are then added dropwise in the course of 1 hour and, after stirring for 3 hours at ambient temperature, the reaction mixture is extracted with ether. The organic phases are washed, dried and concentrated to yield a residue, which is purified by chromatography on silica gel (dichloromethane: 100%) allowing the expected product to be isolated.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06743818B2 |
| Source dataset | uspto-grants-2004_06 |
| ORD ID | ord-434b9a52892548d39ae3ec1eb86718b2 |
| Source note | uspto-grants-2004_06 |