Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | HCID 67672649 | HCID 67672649 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 86753116 | HCID 86753116 | 131.8% |
Reaction Steps
In a 1 L three-neck flask equipped with a stirrer, a thermometer and a reflux condenser, 43.6 g (0.1 mol) of 2,7-bis(bromomethyl)-9-normal-hexylfluorene, 78.7 g (0.3 mol) of triphenylphosphine, and 500 ml of dimethylformamide were introduced and reacted for 12 hours at reflux temperature. When the temperature was decreased to room temperature after reaction, and the reaction solution was dropped down slowly into a 3 L ethylether solvent being thoroughly stirred, to obtain a white solid. After filtering, this solid was washed several times with ethylether, and then dried sufficiently in a vacuum oven at a temperature of 40° C. As a result, 92.2 g (yield: 96%) of a white solid was obtained. [1H-NMR (CDCl3), δ 0.25(br, 3H, CH3), 1.60-1.24(m, 10H, CH2), 2.83(t, 1H, CH), 5.66-5.76(d, 4H, CH2Br), 6.76-7.11(m, 6H, aromatic fluorenyl), 7.49-7.81(m, 30H, aromatic)].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05807974 |
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| Source dataset | uspto-grants-1998_09 |
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| ORD ID | ord-b0379311a0c447debd67d75392e2ba0a |
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| Source note | uspto-grants-1998_09 |
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