Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrogen Peroxide | HCID 784 | — |
| Reactant | Hexane | HCID 8058 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 9-Borabicyclo(3.3.1)nonane | HCID 78966 | — |
| Reactant | HCID 54572837 | HCID 54572837 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 22136233 | HCID 22136233 | — |
Reaction Steps
To a solution of 0.4 M 9-BBN in hexane (72 mL, 28.8 mmol) was added 4-bromophenyl-1-butene (3.99 g, 18.9 mmol) at room temperature. The resulting mixture was stirred at room temperature for 20 h. The mixture was treated sequentially with 3.3 mL of 6N aqueous NaOH (19.8 mmol), THF (7 mL), and 30% H2O2 in H2O (7 mL), then refluxed for 2 h. The reaction mixture was then cooled to room temperature. The organic layer was washed with aqueous sodium sulfite (40 mL), H2O (20 mL), and brine (20 mL). The aqueous extracts were combined, saturated with solid K2CO3 and extracted with Et2O (3×50 mL). The combined organic extracts were dried over Na2 SO4, filtered and concentrated. The resulting crude product was purified by flash chromatography twice (33% EtOAc in hexane and 20% EtOAc in hexane) to yield 4-(o-bromophenyl)butanol).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06777421B2 |
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| Source dataset | uspto-grants-2004_08 |
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| ORD ID | ord-7928864db84e4af482b6b48d347bc933 |
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| Source note | uspto-grants-2004_08 |
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