関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | tert-butyl 4-{1-(2-tetrahydropyranyl)-1H-indazol-5-ylamino}benzoate | HCID 69433104 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 4-(1H-indazole-5-ylamino)benzoic acid | HCID 22933549 | 35% |
反応手順
Trifluoroacetic acid (5 ml) was added to a dichloromethane solution (5 ml) of tert-butyl 4-{1-(2-tetrahydropyranyl)-1H-indazol-5-ylamino}benzoate (205 mg, 0.521 mmol), and the resulting mixture was stirred at room temperature for 3 hours. The mixture was added dropwise to saturated aqueous sodium hydrogencarbonate solution/ethyl acetate and then extracted with ethyl acetate. The extract solution was washed with a saturated aqueous sodium chloride solution, dried over sodium sulfate, and then distilled under reduced pressure to remove the solvent, whereby a crude product was obtained. The crude product was washed by the addition of chloroform containing a small amount of methanol, and then was collected by filtration to obtain 4-(1H-indazole-5-ylamino)benzoic acid (46 mg, 35%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07199147B2 |
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| 出典データセット | uspto-grants-2007_04 |
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| ORD ID | ord-75bc8fcd52144779a7e210772e167b99 |
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| 出典メモ | uspto-grants-2007_04 |
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