참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 2,4-Dichloroaniline | HCID 11123 | — |
| 반응물 | 3-Fluoropyridine-4-carboxylic acid | HCID 345361 | — |
| 반응물 | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 3-[(2,4-Dichlorophenyl)amino]isonicotinic acid | HCID 57649629 | 72% |
반응 단계
2,4-Dichloraniline (162 mg, 1.00 mmol) and 3-fluoropyridine-4-carboxylic acid (141 mg, 1.00 mmol) were dissolved in dry THF (6.0 ml) under argon and the mixture was cooled to −78° C. A solution of LiHMDS (1.0M in THF, 3.5 ml) was added and the reaction mixture was allowed to warm to ambient temperature. After 18 h the reaction was quenched by adding a solution of HCl in dioxane (4.0M, 2.0 ml). The volatiles were removed in vacuo and the crude material was purified by flash chromatography using silica gel and a gradient of 0-10% methanol in DCM as eluent to give 204 mg (721 μmol; 72% yield) of pure desired product.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08524911B2 |
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| 출처 데이터셋 | uspto-grants-2013_09 |
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| ORD ID | ord-1896779e9c5746ddb0e468683b4bf7d2 |
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| 출처 메모 | uspto-grants-2013_09 |
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