참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Toluene | HCID 1140 | — |
| 반응물 | 2-Amino-5-chloropyridine | HCID 66174 | — |
| 반응물 | 5-Chloroisatoic anhydride | HCID 78480 | — |
| 반응물 | Potassium bis(trimethylsilyl)amide | HCID 3251421 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 2-Amino-5-chloro-N-(5-chloropyridin-2-yl)benzamide | HCID 21906418 | 100% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07727982B2 |
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| 출처 데이터셋 | uspto-grants-2010_06 |
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| ORD ID | ord-8d1da3bc63a34c6499333c394caf4bb7 |
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| 출처 메모 | uspto-grants-2010_06 |
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