Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Thiophenol | HCID 7969 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine) | HCID 636044 | — |
| Reactant | HCID 57624605 | HCID 57624605 | — |
| Catalyst | Palladium, tris[mu-[(1,2-eta:4,5-eta)-(1E,4E)-1,5-diphenyl-1,4-pentadien-3-one]]di-, compd. with trichloromethane (1:1) | HCID 11029508 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 57624598 | HCID 57624598 | — |
Reaction Steps
The compound (200 mg) of Example (1-3) was dissolved in 1,4-dioxane (700 μL), and benzenethiol (40 μL), tris(dibenzylideneacetone)dipalladium(0) chloroform adduct (9 mg), 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (Xantphos) (10 mg) and diisopropylethylamine (120 μL) were added. The mixture was stirred at 120° C. for 3 hr. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The extract was washed with water and saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure and the residue was crudely purified by silica gel column chromatography (hexane:ethyl acetate=1:1) to give a mixture (170 mg) as a yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08114902B2 |
|---|
| Source dataset | uspto-grants-2012_02 |
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| ORD ID | ord-3c2994b645f54c728ae851197d50fd0a |
|---|
| Source note | uspto-grants-2012_02 |
|---|
