関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | 2-Amino-5-chloropyridine | HCID 66174 | — |
| 反応物 | 5-Chloroisatoic anhydride | HCID 78480 | — |
| 反応物 | Potassium bis(trimethylsilyl)amide | HCID 3251421 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-Amino-5-chloro-N-(5-chloropyridin-2-yl)benzamide | HCID 21906418 | 100% |
反応手順
To a solution of 2-amino-5-chloropyridine (328 mg, 2.55 mmol) in tetrahydrofuran (5 ml) was 0.5M potassium bis(trimethylsilyl)amide in toluene (10 ml, 5.05 mmol) dropwise at −78° C. After stirred for additional 0.5 hr at −78° C., the mixture was added 5-chloroisatoic anhydride (0.5 g, 2.55 mmol) at −78° C. The mixture was warmed up to r.t gradually and stirred overnight. After quenched by saturated ammonium chloride solution, the mixture was extracted by ethyl acetate. The organic layer was dried over magnesium sulfate and concentrated to give (2-amino-5-chlorophenyl)-N-(5-chloro(2-pyridyl))carboxamide (0.71 g, 100%). MS found for C12H9Cl2N3O M+=282, (M+2)+=284.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07727982B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-8d1da3bc63a34c6499333c394caf4bb7 |
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| 出典メモ | uspto-grants-2010_06 |
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