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Hydrochloric Acid → 3-{[(2,6-Difluorophenyl)amino]sulfonyl}benzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Ethyl 3-{[(2,6-difluorophenyl)amino]sulfonyl}benzoate | HCID 66676178 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-{[(2,6-Difluorophenyl)amino]sulfonyl}benzoic acid | HCID 24422189 | — |
反応手順
To the product of Step A was added ethanol (8 mL) followed by a solution of 50% NaOH (0.96 g, 12.1 mmol) in water (8 mL). The reaction was stirred at ambient temperature for 1.5 hours. To the mixture was added dropwise 1 N HCl (28 mL), and the mixture was stirred at ambient temperature overnight. The solids were collected by filtration, washed with water (2×5 mL), and dried in a vacuum oven at 50° C. overnights to give 3-{[(2,6-difluorophenyl)amino]sulfonyl}benzoic acid: 1H NMR (400 MHz, DMSO-d6) δ ppm 7.11 (t, J=8.1 Hz, 2H), 7.33-7.41 (m, 1H), 7.71 (t, J=7.7 Hz, 1H), 7.92 (dt, J=8.4, 1.1 Hz, 1H), 8.19 (dt, J=7.8, 1.1 Hz, 1H), 8.27 (t, J=1.51 Hz, 1H), 10.20 (s, 1H), 13.48 (s, 1H); MS (ESI) m/z 312 (M−H)−.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08101614B2 |
| 出典データセット | uspto-grants-2012_01 |
| ORD ID | ord-534468a039e447c3aacc634b7b8c66e7 |
| 出典メモ | uspto-grants-2012_01 |