関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Methylglyoxal | HCID 880 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | 2-Aminomalononitrile 4-toluenesulfonate | HCID 18796971 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Methyl 3-methoxy-5-methylpyrazine-2-carboxylate | HCID 21702987 | 27% |
反応手順
Under argon, 5 g (19.3 mmol) of 2-aminomalononitrile-4-toluenesulfonate was initially charged in 50 g of methanol. 4.09 g (22.7 mmol) of sodium methoxide solution (30%) was added and the mixture was stirred at 2° C. for 2 hours. After neutralization with 0.204 g (3.4 mmol) of acetic acid, 3.6 g (19.9 mmol) of methylglyoxal solution (40%) was added. The mixture was stirred at 40° C. for 2 hours and then, at 20° C., 9.2 g (80 mmol) of hydrochloric acid (32%) was added and the mixture was stirred at 20° C. for 6 hours. The solvent was distilled off and the methyl 3-methoxy-5-methylpyrazine-2-carboxylate was extracted with methylene chloride. This gave 1 g of methyl 3-methoxy-5-methylpyrazine-2-carboxylate. The yield was 27 percent. Other data concerning the title product was:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06066736 |
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| 出典データセット | uspto-grants-2000_05 |
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| ORD ID | ord-07967dd299cb4f2fbe524c8cbef10734 |
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| 出典メモ | uspto-grants-2000_05 |
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