関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 3-Bromo-5-iodobenzoic acid | HCID 5182520 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-Bromo-5-hydroxybenzoic acid | HCID 15735511 | — |
反応手順
The title compound was made according to the method described in Org. Proc. Res. Dev. 2002, 6, 591-595. To 5-iodo-3-bromo-benzoic acid (500 mg, 1.53 mmol), NaOH (250 mg, 6.1 mmol), Cu2O (240 mg, 1.68 mmol) was added water (4.0 mL). The mixture was heated for 1.5 h at 140° C. in a sealed tube. The cooled mixture was diluted with water and extracted with CH2Cl2. The aqueous layer was acidified (pH˜2) with TFA and extracted with EtOAc. The organic layer was dried over Na2SO4, filtered, concentrated and purified by reverse-phase HPLC to yield 3-bromo-5-hydroxy-benzoic acid. 1H NMR (400 MHz, DMSO-d6): 10.30 (s, 1H), 7.46 (m, 1H), 7.31 (m, 1H), 7.17 (m, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08476434B2 |
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| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-dd75a7ee621f4db8a2d012ed79effc1b |
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| 出典メモ | uspto-grants-2013_07 |
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