関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 3-(2-Methoxy-ethylamino)-phthalic acid dimethyl ester | HCID 21040133 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3-(2-Methoxy-ethylamino)-phthalic acid | HCID 21988519 | — |
反応手順
To a stirred solution of 3-(2-methoxy-ethylamino)-phthalic acid dimethyl ester (2.24 g, 8.38 mmol) in methanol (50 ml) was added 5N potassium hydroxide (10 ml). The mixture was stirred at room temperature overnight. The solvent was evaporated in vacuo and the residue dissolved in water (50 ml). The water was washed with diethyl ether (2×75 ml). The aqueous portion was cooled in an ice bath and the pH was adjusted to 2–3 by dropwise addition of concentrated hydrochloric acid. The aqueous solution was then extracted with ethyl acetate (3×75 ml). The combined ethyl acetate extracts were washed with brine (100 ml) and dried (MgSO4). The solvent was evaporated in vacuo and the residue, which contained a mixture of diacid and monomethyl esters, was used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07091353B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-4f545cbd274e45a1bffdf54ae55b0fee |
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| 出典メモ | uspto-grants-2006_08 |
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