関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Lithium hydroxide, monohydrate | HCID 168937 | — |
| 反応物 | Methyl 3-((dipropylamino)carbonyl]-5-ethylbenzoate | HCID 22593628 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Methanol tetrahydrofuran water | HCID 21892291 | — |
| 生成物 | 3-[(Dipropylamino)carbonyl]-5-Ethylbenzoic Acid | HCID 22593642 | — |
反応手順
Lithium hydroxide monohydrate (0.0680 g, 1.6 mmol) is added to a mixture of methyl 3-[(dipropylamino)carbonyl]-5-ethylbenzoate (PREPARATION 20, 0.450 g, 1.6 mmol) in a mixture of THF/methanol/water (2/1/1, 8 mL). The mixture is stirred at 20-25 degrees C. for 3 hours. The mixture is then diluted with water (20 mL) and hydrochloric acid (1 N) is added to bring the pH to less than 3. The aqueous mixture is extracted with ethyl acetate. The organic phase is separated and washed with saline, dried over anhydrous magnesium sulfate, filtered and concentrated to give the title compound, MS (ESI+) for C16H23NO3 m/z (M+H)+=278.2.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07727997B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-a595837486be4e039d4224f92ba8f393 |
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| 出典メモ | uspto-grants-2010_06 |
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