関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 1H-Pyrrole-2-carboxylic acid, 3,5-dimethyl-, ethyl ester | HCID 137477 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Methanol tetrahydrofuran water | HCID 21892291 | — |
| 生成物 | 3,5-dimethyl-1H-pyrrole-2-carboxylic acid | HCID 2776468 | 90% |
反応手順
To a solution of ethyl 3,5-dimethyl-2-pyrrolecarboxylate (Aldrich) (504 mg, 3 mmol) in THF/H2O/MeOH (5:1:1, 30 ml) was added NaOH (480 mg, 12 mmol) in H2O (12 ml). The mixture was stirred at 75° C. overnight. The homogeneous mixture was washed with ether. To the aqueous layer was added a saturated aqueous KHSO4 solution until the pH was about 3. The solution was then extracted with dichloromethane. The extracts were dried over MgSO4 and evaporated. The residue was purified on silica (ethylacetate/methanol 90/10) to give the title compound (375 mg, 90%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07528156B2 |
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| 出典データセット | uspto-grants-2009_05 |
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| ORD ID | ord-affd9ab03d1a41febbd17463c5b02f33 |
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| 出典メモ | uspto-grants-2009_05 |
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