関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Hydroxy-[4-(4-isopropyl-piperazine-1-carbonyl)-phenyl]-methanesulfonic acid sodium salt | HCID 59340029 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-(4-Formylbenzoyl)-4-isopropylpiperazine | HCID 57478581 | — |
反応手順
To a suspension of hydroxy-[4-(4-isopropyl-piperazine-1-carbonyl) -phenyl]-methanesulfonic acid sodium salt (49.0 g, 135 mmol) in de-ionized H2O (490 mL) at 0° C. was added 1 N NaOH (100 mL) in 10 mL portions with vigorous stirring. A clear solution resulted (pH 12), which was stirred at 0° C. for 1 h, then at room temperature for 30 min. The aqueous solution was extracted with EtOAc (3×200 mL), followed by CH2Cl2 (3×200 mL). The organic layers were combined, washed with brine (1×300 mL), dried (Na2SO4) and concentrated to yield the title compound as a pale yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07728129B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-0b1125e676684ac0b06b4919e8d322df |
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| 出典メモ | uspto-grants-2010_06 |
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