HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cesium carbonate → HCID 59443069, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | Methanesulfonamide | HCID 72879 | — |
| Reactant | 1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine) | HCID 636044 | — |
| Reactant | HCID 59443040 | HCID 59443040 | — |
| Catalyst | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 59443069 | HCID 59443069 | 57.6% |
Reaction Steps
A mixture of [4-(4-chlorophenyl)-2,2-dimethyl-2H-chromen-7-yl]trifluoromethanesulfonate (100 mg), mesylamine (27 mg), cesium carbonate (117 mg), tris(dibenzylideneacetone)dipalladium (10 mg, 10% wt), 9,9-dimethyl-4,5-bis(diphenylphosphino)-9H-xanthen (Xantphos, 20 mg, 20% wt) and dioxane (2 mL) was heated under reflux for 10 hours. The reaction mixture was filtered, the filtrate was concentrated in vacuo, and the residue was purified by column chromatography on silica gel (petroleum ether/ethyl acetate=100/1) to give the titled compound (50 mg) as a colorless powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08410166B2 |
| Source dataset | uspto-grants-2013_04 |
| ORD ID | ord-a99aa831b70846b28033f7d1f697ef17 |
| Source note | uspto-grants-2013_04 |