Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Pyridine | HCID 1049 | — |
| Edukt | Benzoyl chloride | HCID 7412 | — |
| Edukt | Tetrahydrofuran | HCID 8028 | — |
| Edukt | 9H-Fluorene-9,9-dimethanol | HCID 345022 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | HCID 23125916 | HCID 23125916 | 89% |
Reaktionsschritte
To 11.3 g (0.05 mol) 9,9-dihydroxymethylfluorene was added 50 ml tetrahydrofuran, then added 12.1 ml (0.15 mol) pyridine with stirring. To the resulting homogenous mixture was slowly added 14.5 ml (0.125 mol) benzoyl chloride. The mixture was stirred at room temperature for 1 hour, and then heated refluxing for 4 hours. Upon reaction completion, 70 ml water was added to dissolve the resulting salt. The mixture was extracted with toluene. The organic phase was separated, washed with saturated saline for two times, dried over anhydrous sodium sulfate. The solvent was removed to give a white solid. Recrystallization from ethyl acetate gave 9,9-bis(benzoyloxymethyl)fluorene as a white crystal, the yield was 89%, and m.p. was 144-146° C. 1HNMR: δ (ppm) 4.74(s, 4H, CH2), 7.25-7.75(m, 18H, ArH)
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US07388061B2 |
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| Quelldatensatz | uspto-grants-2008_06 |
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| ORD ID | ord-a7d2e366e4a44ea7acb857e3294796d8 |
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| Quellennotiz | uspto-grants-2008_06 |
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