Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Boric Acid | HCID 7628 | — |
| Reactant | HCID 59297268 | HCID 59297268 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 59297261 | HCID 59297261 | 48% |
Reaction Steps
A mixture N,N′-bis(2-hydroxy-5-methylphenyl)-9,9-dipropyl-3-methoxyfluorene-2,7-dicarboxamide (76.7 g, 0.133 mol), powdered boric acid (1.8 g) and (750 mL) stirred under argon was slowly heated to reflux allowing water to be distilled. After cooling overnight the resulting mixture was further distilled to remove diethylene glycol dibutyl ether (600 mL). The residual mixture was added to methanol (500 mL) causing precipitation of crude product. The mixture was diluted with water (100 mL) and cooled to −20° C. for 18 h. The mixture was filtered and the solid washed with methanol to afford crude product (51.4 g; m. pt. 205-230° C.). Purification by soxhlet extraction with hexane yielded 2,7-Bis(5-methylbenzoxazol-2-yl)-9,9-dipropyl-3-methoxyfluorene (34.6 g; yield 48%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07713452B2 |
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| Source dataset | uspto-grants-2010_05 |
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| ORD ID | ord-6712bf1831b84593ac8cc47a4e7efda0 |
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| Source note | uspto-grants-2010_05 |
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