関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Cyclohexane diethylether | HCID 21895417 | — |
| 反応物 | HCID 23147566 | HCID 23147566 | — |
| 反応物 | HCID 178506676 | HCID 178506676 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | HCID 23147093 | HCID 23147093 | 57% |
反応手順
2-[5-(1,3-Dioxolan-2-yl)furan-2-yl]-3,5-bis(methoxymethoxy)benzaldehyde (135 mg, 0.374 mmol) was dissolved in diethyl ether (10 mL), and the solution was cooled to −78° C., and then cyclohexane/diethyl ether solution of 1.06 mol/L phenyllithium (0.54 mL, 0.57 mmol) was added thereto and stirred at the same temperature for 1 hour. Water was added to the reaction mixture, and extracted with diethyl ether. The organic layer was washed with aqueous saturated sodium chloride solution, then dried over anhydrous sodium sulfate, and the solvent was extracted out under reduced pressure. The resulting residue was purified through preparative thin-layer chromatography (chloroform/methanol=50/1) to obtain 1-{2-[5-(1,3-dioxolan-2-yl)furan-2-yl]-3,5-bis(methoxymethoxy)phenyl}-1-phenylmethanol (93.9 mg, 57%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07538241B2 |
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| 出典データセット | uspto-grants-2009_05 |
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| ORD ID | ord-3e6800d13ea44c318885fbc99d4c9651 |
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| 出典メモ | uspto-grants-2009_05 |
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