Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Phenylboronic Acid | HCID 66827 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 6-Bromoindole | HCID 676493 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | Sodium chloride; water | HCID 57417360 | — |
| Product | 6-phenyl-1H-indole | HCID 13585853 | 45.7% |
Reaction Steps
A solution of 6-bromoindole (2.0 g, 10.20 mmol) in anhydrous toluene (20 mL) under a nitrogen atmosphere was treated with Pd[P(Ph3)]4 (10% mol). After stirring the mixture for 30 min., phenylboronic acid (1.87 g, 15.30 mmol) in anhydrous EtOH (10 mL) was added followed by the addition of sat'd NaHCO3 (6 mL). The bi-phasic mixture was heated to reflux for 24 h. After cooling to room temperature, the mixture was added to a sat'd brine solution and extracted with EtOAc (2×). The organic layer was dried over MgSO4, filtered and concentrated in vacuo. The residue was purified by flash column chromatography (1:1 CH2Cl2/heptane) to give the desired material as white powder (900 mg, 45%): 1H NMR (DMSO-d6, 300 MHz) δ 11.15 (br s, 1H), 7.58-7.66 (m, 4H), 7.41-7.47 (m, 2H), 7.36 (m, 1H), 7.26-7.31 (m, 2H), 6.42 (m, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07304079B2 |
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| Source dataset | uspto-grants-2007_12 |
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| ORD ID | ord-9447cfbfb29b445a9691b5dade34ab4a |
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| Source note | uspto-grants-2007_12 |
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