関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Lithium Hydroxide | HCID 3939 | — |
| 反応物 | 1,4-Dioxane | HCID 31275 | — |
| 反応物 | Ethyl 5-(trifluoromethyl)-1-[6-(2-{[4'-(trifluoromethyl)biphenyl-4-yl]methoxy}phenyl)pyridin-2-yl]-1H-pyrazole-4-carboxylate | HCID 86633489 | — |
| 生成物 | Trifluoroacetic acid | HCID 6422 | — |
| 生成物 | 5-(Trifluoromethyl)-1-[6-(2-{[4'-(trifluoromethyl)biphenyl-4-yl]methoxy}phenyl)pyridin-2-yl]-1H-pyrazole-4-carboxylic acid | HCID 25233126 | — |
反応手順
To a solution of the title compound from Example 2 Step B (ca. 0.073 mmol) in 1,4-dioxane (0.5 mL) was added lithium hydroxide (0.50 mL, 2.0 M in water, 1.00 mmol), and the resulting mixture was stirred at 50° C. After 2 h, the reaction mixture was rendered acidic by addition of aqueous hydrochloric acid, then was diluted with 1,4-dioxane and passed through a 0.45 micron syringe filter. Purification by reverse phase HPLC (50 to 100% acetonitrile in water, each with 0.1% v/v TFA) provided the title compound: LCMS m/z 584.1 [M+H]+; 1H NMR (500 MHz, d6-DMSO) δ 8.30 (s, 1H), 8.18 (d, J=8.0 Hz, 1H), 8.14 (t, J=8.0 Hz, 1H), 7.88 (d, J=8.0 Hz, 2H), 7.80 (d, J=8.0 Hz, 2H), 7.75-7.71 (m, 4H), 7.56 (d, J=8.0 Hz, 2H), 7.46-7.43 (m, 1H), 7.30 (d, J=7.5 Hz, 1H), 7.11 (t, J=7.5 Hz, 1H), 5.32 (s, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08455638B2 |
|---|
| 出典データセット | uspto-grants-2013_06 |
|---|
| ORD ID | ord-f239249ca43d402692c0c2102c59376c |
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| 出典メモ | uspto-grants-2013_06 |
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