HuagongsheHuagongshe Chemistry Print Report · For research reference only
Iodobenzene → HCID 57860210, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Iodobenzene | HCID 11575 | — |
| Reactant | 2-Dicyclohexylphosphino-2',4',6'-triisoprophylbiphenyl | HCID 11155794 | — |
| Reactant | Sodium t-butoxide | HCID 23676156 | — |
| Reactant | HCID 57860479 | HCID 57860479 | — |
| Catalyst | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | tert-Butanol | HCID 6386 | — |
| Product | HCID 57860210 | HCID 57860210 | 30% |
Reaction Steps
A solution of the compound of Example 77 (200 mg, 0.42 mmol), iodobenzene (0.50 mL), tris(dibenzylideneacetone)dipalladium (0) (38 mg, 0.042 mmol), x-phos (40 mg, 0.085 mmol) and sodium tert-butoxide (102 mg, 1.1 mmol) in tert-butanol (4.0 mL) was stirred under microwave irradiation at 130° C. for 35 min. The reaction mixture was diluted with water, and extracted twice with ethyl acetate. The extracts were combined, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was purified by aminosilica gel chromatography (eluate; ethyl acetate/hexane=30/70-100/0) and recrystallized from ethyl acetate to give the title compound (70 mg, 30%) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08399449B2 |
| Source dataset | uspto-grants-2013_03 |
| ORD ID | ord-d9c2e75b8c044bcfb33748c36807d6df |
| Source note | uspto-grants-2013_03 |