関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Methyl 2-bromo-4-methylbenzoate | HCID 21779704 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | Methyl 2-bromo-5-iodo-4-methylbenzoate | HCID 69844638 | 89.6% |
反応手順
To a round-bottom flask was added a mixture of methyl 2-bromo-4-methylbenzoate (2.00 g, 7.86 mmol, 1.00 equiv) in AcOH (20 mL). I2 (2.45 g, 9.65 mmol, 1.10 equiv), NaIO4 (950 mg, 4.42 mmol, 0.50 equiv), and sulfuric acid (0.1 mL, 0.15 equiv) were added and the resulting mixture was stirred at 100° C. overnight. After cooling to ambient temperature, the reaction was carefully quenched with Na2S2O3 (aq., sat.). The resulting mixture was extracted with 2×50 mL of ethyl acetate. The combined organic layers were dried (Na2SO4) and concentrated in vacuo to yield 2.50 g (81%) of the title compound as an off-white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08871790B2 |
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| 出典データセット | uspto-grants-2014_10 |
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| ORD ID | ord-e045711f0c8648bfb6adecd963342007 |
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| 出典メモ | uspto-grants-2014_10 |
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