참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Tetrahydrofuran | HCID 8028 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 3-Chloropyridin-4-amine | HCID 581853 | — |
| 반응물 | 5-(4-Methyl-5-trifluoromethyl-isoxazol-3-yl)-thiophene-2-carboxylic acid | HCID 25210997 | — |
| 용매 | Pyridine | HCID 1049 | — |
| 생성물 | HCID 25211383 | HCID 25211383 | 83% |
반응 단계
Prepared from 5-(4-Methyl-5-trifluoromethyl-isoxazol-3-yl)-thiophene-2-carboxylic acid and 4-amino-3-chloropyridine by the method described in Example 2 Method B reversing the order of addition such that solid acid chloride was added to a THF solution of triethylamine and pyridine derivative. The reaction mixture was evaporated to a solid, triturated and filtered with the aid of water, then washed with a saturated aqueous NaHCO3 solution followed by water to afford product as a colorless solid (80 mg, 83%). 1H NMR (CDCl3) 2.40 (s, 3H), 7.59 (d, J=4.0, 1H), 7.73 (d, J=4.0, 1H), 8.46 (s, 3H), 8.59 (s, 1H). 13C NMR 7.9, 114.5, 114.7, 118.6 (q, J=271), 129.0, 129.7, 135.2, 140.4, 141.0, 149.4, 149.6, 155.6 (q, J=40), 157.6, 159.3. 19F NMR −63.1. LC/MS 6.68 min, [M+1]+388.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09029397B2 |
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| 출처 데이터셋 | uspto-grants-2015_05 |
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| ORD ID | ord-c3b59be973e24c87aa20399b41946ea3 |
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| 출처 메모 | uspto-grants-2015_05 |
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