関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Isobutyryl chloride | HCID 62325 | — |
| 反応物 | 3-Amino-5-bromopyridine | HCID 817681 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-(5-bromopyridin-3-yl)-2-methylpropanamide | HCID 68195778 | 71% |
反応手順
3-Amino-5-bromo pyridine (XXX) (1 eq) was dissolved in DCM and cooled to 0° C. before adding pyridine (2.2 eq) and isobutyryl chloride (XXXI) (1.1 eq). The reaction mixture was stirred at r.t. for 15 h until TLC showed the reaction was complete. The reaction mixture was diluted with DCM and washed with water. The organic extract was dried, concentrated and purified by column chromatography using silica gel (100-200 mesh) to afford N-(5-bromopyridin-3-yl)isobutyramide (XXXII) as a off white solid, (71% yield). 1H NMR (CDCl3) δ ppm 8.55-8.35 (m, 3H), 7.32 (s, 1H), 2.59-2.48 (m, 1H), 1.28-1.27 (d, 6H); ESIMS found C9H11BrN2O m/z 243.05(M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08846714B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-e2d0f47f2cd0488b90a841ec61e944bf |
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| 出典メモ | uspto-grants-2014_09 |
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