関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | HCID 21882727 | HCID 21882727 | — |
| 反応物 | 5-Iodopyridine-2,3-diamine | HCID 21882766 | — |
| 生成物 | HCID 178493175 | HCID 178493175 | 61.2% |
反応手順
With stirring, a mixture of 8.06 g of 3-(4-methoxypyridin-2-yl)propionic acid (starting material B1), 9.5 g of 2,3-diamino-5-iodopyridine (Cugola et al., Bioorg.Med. Chem.Let 22, 2749-2754 (1996)) and 150 g of polyphosphoric acid (PPA) is heated at 140° C. for 22 hours. After cooling, the mixture is poured into about 1000 ml of ice-water and then neutralized (pH 7-8) using 6N aqueous sodium hydroxide solution. The mixture is extracted four times with ethyl acetate and the combined organic phases are evaporated to dryness. The residue is crystallized first from ethyl acetate and then from methanol, giving 9.4 g of the title compound as a light-beige powder of m.p. 207-208° C.; the mass spectrum shows the molecular peak MH+ at 381.2 Da.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07279488B2 |
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| 出典データセット | uspto-grants-2007_10 |
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| ORD ID | ord-c298ddac61494c26a2c67a3b9ecc2d5b |
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| 出典メモ | uspto-grants-2007_10 |
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