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Lithium Hydroxide → 1-(4-Methoxyphenyl)-3-methylthio-1H-pyrazole-5-carboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Lithium Hydroxide | HCID 3939 | — |
| 反応物 | methyl 1-(4-methoxyphenyl)-3-methylthio-1H-pyrazole-5-carboxylate | HCID 18177273 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 1-(4-Methoxyphenyl)-3-methylthio-1H-pyrazole-5-carboxylic acid | HCID 18177301 | 98.9% |
反応手順
A solution of lithium hydroxide (4.5 mL, 1.0 M, 4.5 mmol) was added to a suspension of methyl 1-(4-methoxyphenyl)-3-methylthio-1H-pyrazole-5-carboxylate (840 mg, 3.0 mmol) in MeOH (30 mL) and stirred at room temperatureerature for 21 hours. The resulting mixture was concentrated and partitioned between EtOAc and H2O. The organic layer was removed, and the aqueous layer was acidified with 1M HCl and extracted twice with EtOAc. The combined organic extracts were dried over Na2SO4, filtered, and evaporated to yield clean product (784 mg, 98%). 1H NMR (CDCl3): δ7.33 (d, 2H, J=8.4), 6.97 (s, 1H), 6.95 (d, 2H, J=8.4), 3.85 (s, 3H), 2.55 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06403620B1 |
| 出典データセット | uspto-grants-2002_06 |
| ORD ID | ord-dc39abd683fd46579c0c776c93bf457b |
| 出典メモ | uspto-grants-2002_06 |