関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Chloride | HCID 5234 | — |
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Benzoic acid, 2-hydroxy-3-methyl-, methyl ester | HCID 31835 | — |
| 反応物 | Sodium Hypochlorite | HCID 23665760 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Hydroxy-5-iodo-3-methylbenzoic acid | HCID 15908685 | — |
反応手順
14.9 mL (24.1 mmol) sodium hypochlorite solution (10 percent by weight in water) is added dropwise to a solution of 4.0 g (24.1 mmol) methyl 2-hydroxy-3-methyl-benzoate, 3.6 g (24.1 mmol) NaI, 0.96 g (24.1 mmol) NaOH in 100 mL MeOH at −5° C. over 40 min. The reaction is stirred for 30 min at −5° C. and 5 days at RT. The solvent is eliminated i.vac. and the residue is taken up in 80 mL water and 50 mL DCM. After the organic phase has been saturated with NaCl it is extracted twice with DCM. The combined organic extracts are filtered and the solvent is eliminated i.vac. The product is further reacted without any more purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08618132B2 |
|---|
| 出典データセット | uspto-grants-2013_12 |
|---|
| ORD ID | ord-638b86c89d4a4a29b79d882457ac8a43 |
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| 出典メモ | uspto-grants-2013_12 |
|---|
