関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Diisobutylaluminumhydride | HCID 21225700 | — |
| 反応物 | Methyl 3-bromo-5-iodobenzoate | HCID 21942573 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (3-Bromo-5-iodophenyl)methanol | HCID 15467379 | 96.7% |
反応手順
To methyl 5-bromo-3-iodobenzoate (Step A above) (5.01 g, 0.015 mole) in anhydrous methylene chloride (100 mL) at -78° C., was added dropwise minutes, diisobutylaluminum hydride (5.50 mL, 0.03 mole). The mixture was stirred for 1 hour then allowed to warm to 0° C. The reaction solution was poured into 600 mL, chilled 3N HCl and extracted 3× with methylene chloride (150 mL). The organic layers were combined, dried over MgSO4 and concentrated under vacuum to yield 5-bromo-3-iodobenzyl alcohol (4.54 g) as a white solid. MP=110-112° C. MS and NMR were consistent with the desired structure.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06028223 |
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| 出典データセット | uspto-grants-2000_02 |
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| ORD ID | ord-7a3136ee0bb84c16864a250cede4929f |
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| 出典メモ | uspto-grants-2000_02 |
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