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HRID 1091669作成日:2026年10月27日
Potassium Carbonate → 2-[6-carboxybenzothiazol-2(3H)-ylidene]-2-(4-trifluoromethyl-pyrimidin-2-yl)acetonitrile
https://huagongshe.com/reaction/1091669
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Amino-3-mercaptobenzoic acid | HCID 598058 | — |
| 反応物 | 3,3-Bis(methylthio)-2-(4-trifluoromethylpyrimidin-2-yl)acrylonitrile | HCID 86640517 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-[6-carboxybenzothiazol-2(3H)-ylidene]-2-(4-trifluoromethyl-pyrimidin-2-yl)acetonitrile | HCID 66593546 | 44.5% |
反応手順
A mixture of 4-amino-3-mercaptobenzoic acid (768 mg, 4.5 mmol), 3,3-bis(methylthio)-2-(4-trifluoromethylpyrimidin-2-yl)acrylonitrile (1.45 g, 5.0 mmol, 1.1 eq.), 4-dimethylaminopyridine (550 mg, 4.5 mmol, 1 eq.), and potassium carbonate (622 mg, 4.5 mmol, 1 eq.) in ethanol (20 mL) was heated at 160° C. for 0.4 hr in a microwave. The mixture was cooled to room temperature, diluted with DCM, and washed with 1M hydrochloric acid. The DCM fraction was decanted, filtered, and concentrated under vacuum to give 2-[6-carboxybenzothiazol-2(3H)-ylidene]-2-(4-trifluoromethyl-pyrimidin-2-yl)acetonitrile (729 mg, 40% yield) as a brown solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08129396B2 |
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| 出典データセット | uspto-grants-2012_03 |
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| ORD ID | ord-b32016c9a04f42898ca8ce3fbc4e6282 |
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| 出典メモ | uspto-grants-2012_03 |
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