関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 4-Chloro-N-(4-(methylthio)phenyl)benzothioamide | HCID 57617480 | — |
| 触媒 | Potassium ferricyanide | HCID 26250 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-(4-Chlorophenyl)-6-(methylthio)benzo[d]thiazole | HCID 57617482 | 67.2% |
反応手順
To a solution of potassium hexacyanoferrate(III) (670 mg, 2.04 mmol) in water (5 mL) at 90° C. was added dropwise over 5 minutes a solution of 4-chloro-N-(4-(methylthio)phenyl)benzothioamide (150 mg, 0.51 mmol) in ethanol (2 mL) and 3M aqueous sodium hydroxide solution (1.4 mL, 4.08 mmol). The resulting mixture was heated at 90° C. for 30 minutes. After cooling, the precipitate formed was filtered off and washed with water to give a yellow solid. The yellow solid was purified by column chromatography eluting using a gradient (hexanes to ethyl acetate/hexanes 5:95 v/v) to afford 100 mg (67%) of the title compound (LCMS RT=9.37 min, MH+ 292.2)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08501713B2 |
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| 出典データセット | uspto-grants-2013_08 |
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| ORD ID | ord-882ebaf4bfc04662932e623e0eb3216e |
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| 出典メモ | uspto-grants-2013_08 |
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