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Water → (2-Iodo-4-nitrophenyl)methanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Methyl 2-iodo-4-nitrobenzoate | HCID 232745 | — |
| 反応物 | Lithium borohydride | HCID 4148881 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | (2-Iodo-4-nitrophenyl)methanol | HCID 279258 | 67% |
反応手順
To a solution of methyl 2-iodo-4-nitrobenzoate (25.6 g, 83.4 mmol) in THF (400 mL) was added lithium tetrahydroborate (2.2 g, 92 mmol). The reaction solution was stirred at rt for 2 h and cooled down to 0° C., and water was added dropwise. After stirring for 10 min, ethyl acetate was added. The organic solution was separated and washed with brine, dried over Na2SO4, filtered and concentrated. The residue was purified with flash chromatography (30% ethyl acetate/hexs) to give the desired product as yellow solid (15.6 g, 67%). LCMS calculated for C7H71NO3(M+H)+: m/z=280.0.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08871753B2 |
| 出典データセット | uspto-grants-2014_10 |
| ORD ID | ord-2e76ffa7ba754aa7b26495467834c37d |
| 出典メモ | uspto-grants-2014_10 |