Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Boron tribromide | HCID 25134 | — |
| Reactant | HCID 68864000 | HCID 68864000 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 68864367 | HCID 68864367 | 76.9% |
Reaction Steps
Boron tribromide (1 M dichloromethane solution: 6.00 ml) was added dropwise to a mixture of the compound of Example 31 (0.86 g) and dichloromethane (20 ml) at 0° C., and the mixture was stirred at 25° C. overnight. Water was added to the reaction solution. The thus-precipitated crystals were collected by filtration, purified by silica gel column chromatography (eluent: ethyl acetate/hexane=1/3), and recrystallized from ethanol, thereby giving 0.64 g of the desired compound. Melting point: 243-245° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07514452B2 |
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| Source dataset | uspto-grants-2009_04 |
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| ORD ID | ord-8a64ae8b162f431c80977dbbd6bb271b |
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| Source note | uspto-grants-2009_04 |
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