関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Ethyl (E)-3-(6-amino-4-methylpyridin-3-yl)acrylate | HCID 57440845 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | (E)-3-(6-Amino4-methylpyridin-3-yl)acrylic acid HCl salt | HCID 67343018 | — |
反応手順
To ethyl (E)-3-(6-amino-4-methylpyridin-3-yl)acrylate (1.50 g, 7.3 mmole) was added HOAc (15 mL) and conc. HCl (15 mL). The solution was stirred at 100° C. for 10 hr, cooled to RT, and concentrated to dryness. Trituration with Et2O, filtration and drying under vacuum gave the title compound (1.65 g, quantitative) as a white solid: LCMS (ES) m/e 179.2 (M+H)+; 1H NMR (400 MHz, DMSO-d6) δ 8.37 (s,1H), 8.28 (br s, 3H), 7.51 (d, I=16.0 Hz,1H), 6.86 (s,1H), 6.46 (d, J=16.0 Hz,1H), 2.41 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06846819B1 |
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| 出典データセット | uspto-grants-2005_01 |
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| ORD ID | ord-024ee6a331b844788d9b8b7999b46d69 |
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| 出典メモ | uspto-grants-2005_01 |
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