関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | 3-Hydroxybenzoic Acid | HCID 7420 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Sodium Hypochlorite | HCID 23665760 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3-Hydroxy-4-iodobenzoic acid | HCID 736854 | 31.8% |
反応手順
21 g (520 mmol) of sodium hydroxide and then 78.7 g (520 mmol) of sodium iodide are added to a solution of 69 g (500 mmol) of 3-hydroxybenzoic acid in 700 mL of methanol. The reaction mixture is cooled to 0° C. and aqueous sodium hypochlorite solution is then added (520 mmol). The reaction medium is stirred at 0-5° C. for 2 hours and then at room temperature overnight. The methanol is evaporated off and the reaction medium is then acidified with concentrated hydrochloric acid solution. The precipitated product is filtered off, washed with water and dried. 41.92 g of 3-hydroxy-4-iodobenzoic acid are obtained in the form of an off-white solid. The aqueous phase is extracted with ethyl acetate, dried over magnesium sulfate, filtered and evaporated and the residue obtained is taken up in heptane and then filtered.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08383652B2 |
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| 出典データセット | uspto-grants-2013_02 |
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| ORD ID | ord-e3f504ac44c9462b9c0bd6996b66d575 |
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| 出典メモ | uspto-grants-2013_02 |
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