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Hydrochloric Acid → 6-Methoxy-3-pyridineacetic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | HCID 59750617 | HCID 59750617 | — |
| 溶媒 | Sodium hydroxide tetrahydrofuran | HCID 20445995 | — |
| 生成物 | 6-Methoxy-3-pyridineacetic acid | HCID 11953492 | — |
反応手順
2-(6-Methoxy-pyridin-3-yl)-malonic acid diethyl ester (5.6 g, 21.0 mmoL) prepared in Example 3 was dissolved in 2N NaOH/THF:H2O (1:1) (20 mL). The resulting mixture was heated to reflux for 3 hours. The reaction mixture was then adjusted to pH=1 by concentrated HCl and stirred at room temperature for another 1 hour. The solution was then adjusted to pH=13 by 1N NaOH and extracted with ether. The aqueous phase was acidified to pH=5 by 1N HCl and extracted 3× by ethyl acetate. The combined organic phase was then washed with brine, dried over anhydrous Na2SO4, filtered and concentrated to give the title compound a white solid (2.45, 70%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07399767B2 |
| 出典データセット | uspto-grants-2008_07 |
| ORD ID | ord-d0fdc75ef94e4a17bdaafe818acaffdb |
| 出典メモ | uspto-grants-2008_07 |