関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2-Bromobenzenethiol | HCID 80598 | — |
| 反応物 | 5-Carboxy-2-fluorobenzenesulfinic acid | HCID 10679678 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-(2-Bromo-phenylsulfanyl)-3-sulfino-benzoic Acid | HCID 22139410 | — |
反応手順
2-Bromobenzenethiol (25 g, 132 mmol) was added to a solution of 4-fluoro-3-sulfino-benzoic acid (13.5 g, 66 mmol) and NaOH pellets (11 g, 264 mmol) in water (30 ml). The yellow mixture was then degassed for 10 minutes and then heated to 140° C. for 48 hours. The reaction was then cooled to 0° C. and acidified to pH 4-5 (pH paper) with concentrated HCl. The precipitate formed was filtered, washed with hexane and was dried in a vacuum dessicator over activated silica overnight (20.69 g, 84%). m/z (LC-MS, ESP), RT=3.67 min, M−−1)=373.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07429660B2 |
|---|
| 出典データセット | uspto-grants-2008_09 |
|---|
| ORD ID | ord-667e20ec9f2246dd8df81440fb1cb236 |
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| 出典メモ | uspto-grants-2008_09 |
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