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Sodium Hydroxide → HCID 58425466、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 5-tert-Butyl-4-fluoro-2-methyl-2H-pyrazole-3-carboxylic acid ethyl ester | HCID 67413334 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | HCID 58425466 | HCID 58425466 | — |
反応手順
5-tert-Butyl-4-fluoro-2-methyl-2H-pyrazole-3-carboxylic acid ethyl ester (61.4 mg, 0.269 mmol, prepared as described in the previous step) was dissolved in MeOH (1 mL) then 2 M NaOH (175 μL, 0.350 mmol) was added. The resulting mixture was stirred at room temperature for 18 h and the solvent was removed under reduced pressure. The resulting residue was dissolved in H2O (10 mL) and acidified to pH˜2 using 3 M HCl. The aqueous layer was extracted with DCM (3×5 mL), the combined organic extracts were dried over MgSO4 and filtered. The solvent was removed under reduced pressure to yield 5-tert-Butyl-4-fluoro-2-methyl-2H-pyrazole-3-carboxylic acid. 1H-NMR H-NMR (400 MHz, CDCl3) δ: 9.89 (br. s., 1H), 4.06 (d, J=1.0 Hz, 3H), 1.36 (s, 9H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09023846B2 |
| 出典データセット | uspto-grants-2015_05 |
| ORD ID | ord-62394332cd7b4a29b35fc7842dfca5be |
| 出典メモ | uspto-grants-2015_05 |