HuagongsheHuagongshe Chemistry Print Report · For research reference only
Bis[2-(diphenylphosphino)phenyl] ether → HCID 57763231, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Bis[2-(diphenylphosphino)phenyl] ether | HCID 4285986 | — |
| Reactant | Benzenethiol, 4-[[(1,1-dimethylethyl)dimethylsilyl]oxy]- | HCID 11701480 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Reactant | HCID 57763225 | HCID 57763225 | — |
| Catalyst | Tris(dibenzylideneacetone) dipalladium | HCID 9832798 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 57763231 | HCID 57763231 | 46.4% |
Reaction Steps
A stirred mixture of Intermediate 37 (0.8 g) and 4-{[tert-butyl(dimethyl)silyl]oxy} benzenethiol (0.74 g, EP465802A1), with (oxydi-2,1-phenylene)bis(diphenylphosphine) (0.05 g), potassium tert-butoxide (0.26 g) and tris(dibenzylideneacetone) dipalladium(0) (0.08 g) in toluene (30 ml) was heated at 106° C. for 18 h. The mixture was cooled, diluted with ethyl acetate (25 ml) and washed with a sodium carbonate solution (30 ml). The organic extracts were washed with water (30 ml) , dried (Na2SO4) and concentrated in vacuo. The residue was purified by chromatography on silica gel using ethyl acetate/diethyl ether (7:3) as the eluent. The appropriate fractions were concentrated in vacuo to give the title compound as a yellow foam (0.38 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07566786B2 |
| Source dataset | uspto-grants-2009_07 |
| ORD ID | ord-b6f28e2cc1304101b966e5107ae9d6a1 |
| Source note | uspto-grants-2009_07 |