関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Methyl 6-iodo-2-phenylpyrazolo[1,5-a]pyridine-3-carboxylate | HCID 59233743 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Lithium Hydroxide | HCID 3939 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 6-Iodo-2-phenylpyrazolo[1,5-a]pyridine-3-carboxylic acid | HCID 59233771 | 85% |
反応手順
Methyl-6-iodo-2-phenylpyrazolo[1,5-a]pyridine-3-carboxylate (250 mg, 0.661 mmol) was dissolve in aqueous LiOH(2N,1 mL), methanol (2 mL) and tetrahydrofuran (7 mL). This solution was stirred overnight at 45° C. After 24 hours, 2 mL 2M LiOH and 2 mL methanol were added. Heated at 55° C. overnight. The reaction was cooled on an ice water bath and aqueous hydrochloric acid (10 mL, 1N) was added dropwise until acidic by pH paper. Ethylacetate (200 mL) and water (40 mL) were added. The organic portion was extracted with brine (20 mL) and was dried over magnesium sulfate. The solvent was removed by rotory evaporation. The residue was place under vacuum overnight to give of a white solid (204 mg, 85%). 1H NMR (500 MHz, DMSO-D6) δ ppm 7.47 (m, 3H) 7.77 (m, 2H) 7.97 (d, J=9.46 Hz, 1H) 9.27 (s, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08536338B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-ebd467546d364a949bbc9bec91c6b6a0 |
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| 出典メモ | uspto-grants-2013_09 |
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