関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methane | HCID 297 | — |
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | methyl 2(R)-[[4-methoxybenzenesulfonyl](3-picolyl)-amino]-3-methylbutanoate hydrochloride | HCID 22856285 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2(R)-[[4-methoxybenzenesulfonyl](3-picolyl)amino]-3-methyl-butanoic acid hydrochloride | HCID 70061703 | — |
反応手順
Methyl 2(R)-[[4-methoxybenzenesulfonyl](3-picolyl)amino]-3-methylbutanoate hydrochloride (7164 g, 16.7 mol) is added to a solution of water (27 L) and concentrated hydrochloric acid (9 L), and heated to 120° C. for 3 days. After cooling down to room temperature, charcoal (350 g) is added, stirring is continued for 45 minutes, the reaction is filtered, and the solvent is evaporated. The crude solid is re-dissolved in methanol (7.1 L) and ethyl acetate (73 L), and cooled to 3° C. for 2 hours. The precipitated product is collected by filtration to give 2(R)-[[4-methoxybenzenesulfonyl](3-picolyl)amino]-3-methylbutanoic acid hydrochloride.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05646167 |
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| 出典データセット | uspto-grants-1997_07 |
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| ORD ID | ord-c70488d5ae7f4cb79e0249a2fc5f67b7 |
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| 出典メモ | uspto-grants-1997_07 |
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