Participants
| Role | Name | HCID | Charge |
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| Reactant | Boron tribromide | HCID 25134 | — |
| Reactant | HCID 86584085 | HCID 86584085 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86584086 | HCID 86584086 | 51.1% |
Reaction Steps
To a solution of the title compound from Step C (26 mg, 0.060 mmol) in dichloromethane (1 ml) at room temperature was added boron tribromide (1M in dichloromethane, 0.12 ml, 0.12 mmol). After the addition, a brown solution was obtained which was stirred at room temperature for about three hours. An additional 4 equivalents of boron tribromide was added and the mixture was stirred for 15 minutes at room temperature. A brown precipitation formed. The reaction was quenched with water (5 ml) and extracted with dichloromethane (3×10ml). The combined extracts were dried, filtered, and concentrated, and the residue was purified by preparative TLC (7% methanol in dichloromethane) to give the title compound (13 mg) as an off-white solid. MS (APCl−) Calc: 423.0, Found: 422.0 (M−1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06620830B2 |
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| Source dataset | uspto-grants-2003_09 |
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| ORD ID | ord-3fc40aacce2740eca5c69d5da9164d3d |
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| Source note | uspto-grants-2003_09 |
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