関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diisobutylaluminum hydride | HCID 14487 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Benzoic acid, 4-iodo-2-methoxy-, methyl ester | HCID 22619468 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-Iodo-2-methoxybenzyl alcohol | HCID 18779792 | 31.2% |
反応手順
A solution of methyl 4-iodo-2-methoxybenzoate (840 mg, 2.88 mmol) in THF was purged with nitrogen and cooled to −78° C. DIBALH (6 mL, 5.75 mmol, 1M in toluene) was added slowly. The mixture was then stirred at the same temperature for an hour. Saturated aqueous NH4Cl solution was added, followed by extraction with ethyl acetate twice. The organic phase was then washed with brine and dried with anhydrous Na2SO4. Solvent was removed and the resulting residue purified by flash column chromatograph to give 237 mg of the title compound (31%). 1H NMR (400 MHz, CDCl3): δ 2.17 (1H, s), 3.84 (3H, s), 4.62 (2H, d, J=4.0 Hz), 7.01 (1H, d, J=7.6 Hz), 7.18 (1H, s), 7.29 (1H, d, J=8.0 Hz).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09107916B2 |
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| 出典データセット | uspto-grants-2015_08 |
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| ORD ID | ord-1d531f9b47474f1b86623a248e6a9531 |
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| 出典メモ | uspto-grants-2015_08 |
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