関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Benzoyl chloride | HCID 7412 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | 9H-Fluorene-9,9-dimethanol | HCID 345022 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 9,9-Bis(benzoyloxymethyl)fluorene | HCID 23125916 | 89% |
反応手順
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)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07388061B2 |
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| 出典データセット | uspto-grants-2008_06 |
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| ORD ID | ord-a7d2e366e4a44ea7acb857e3294796d8 |
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| 出典メモ | uspto-grants-2008_06 |
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