Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Boron tribromide | HCID 25134 | — |
| Reactant | HCID 90979974 | HCID 90979974 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 91520096 | HCID 91520096 | 49.7% |
Reaction Steps
Boron tribromide (1 M dichloromethane solution: 12.00 ml) was added dropwise to a dichloromethane (5 ml) solution of the compound of Example 84 (0.86 g) at 0° C., and stirred overnight at 25° C. After water was added to the reaction solution, the thus-precipitated crystals were filtered and purified by silica gel column chromatography (eluent: methanol/chloroform=1/9), thereby giving 0.40 g of the desired compound. Melting point: 168-172° C. (Recrystallized from ethyl acetate)
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-d157771898304dccaf9e6e9402454460 |
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| Source note | uspto-grants-2009_04 |
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