Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethylenediamine | HCID 3301 | — |
| Reactant | Sodium Iodide | HCID 5238 | — |
| Reactant | 4-Bromobiphenyl | HCID 7101 | — |
| Reactant | Sulfolane | HCID 31347 | — |
| Catalyst | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| Solvent | Hexane | HCID 8058 | — |
| Product | 4-Iodobiphenyl | HCID 15322 | 94% |
Reaction Steps
A Schlenk tube was charged with CuI (19.5 mg, 0.102 mmol, 10 mol %), 4-bromobiphenyl (234 mg, 1.00 mmol), NaI (300 mg, 2.00 mmol), evacuated and backfilled with argon. Ethylenediamine (13.5 μL, 0.202 mmol, 20 mol %) and sulfolane (1.0 mL) were added under argon. The Schlenk tube was sealed with a Teflon valve and the reaction mixture was stirred at 130° C. for 23 h. The resulting suspension was allowed to reach room temperature, poured into hexane (20 mL) and washed with water (3×20 mL). The combined organic phases were dried (MgSO4), concentrated, and the residue was purified by flash chromatography on silica gel (hexane) to provide 262 mg (94% yield) of 4-iodobiphenyl as white crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US06888032B2 |
|---|
| Source dataset | uspto-grants-2005_05 |
|---|
| ORD ID | ord-1d0c577069ab40c49f7e943d629e86ed |
|---|
| Source note | uspto-grants-2005_05 |
|---|