関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | Methyl 6-chloro-2-methylpyridine-3-carboxylate | HCID 59650775 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | tert-Butanol | HCID 6386 | — |
| 生成物 | 6-Chloro-2-methylpyridine-3-carboxylic acid | HCID 46223839 | — |
反応手順
Methyl 6-chloro-2-methylnicotinate (Example 423, Step 2) (900 mg, 4.85 mmol) was taken up in 2-methylpropan-2-ol (48.5 ml) and methanol (48.5 ml) and aqueous 1 molar potassium hydroxide (24.2 ml, 24.2 mmol) was added. The resulting slurry was heated at 60° C. for 4 hours, cooled to room temperature, and hydrochloric acid (1 M in water, 24.2 mL, 24.2 mmol) was added dropwise. The solution was then concentrated under reduced pressure until to afford a white solid, which was taken up in methanol and concentrated under reduced pressure. Water and ethyl acetate were added and the layers were separated. The aqueous layer was extracted with ethyl acetate three times. The combined organic layers were concentrated under reduced pressure to afford the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08367706B2 |
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| 出典データセット | uspto-grants-2013_02 |
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| ORD ID | ord-0c35258874e645b892156fe40896f9a9 |
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| 出典メモ | uspto-grants-2013_02 |
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