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Lithium hydroxide, monohydrate → 2-Isobutylsuccinic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Lithium hydroxide, monohydrate | HCID 168937 | — |
| 反応物 | 2-Isobutylsuccinic acid 1-methyl ester | HCID 10130288 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 2-Isobutylsuccinic acid | HCID 3031825 | 53.1% |
反応手順
A solution of lithium hydroxide monohydrate (26 mg, 0.61 mmol) in water (250 μl) was added to a stirred solution of (2R) 2-isobutylsuccinic acid 1-methyl ester (100 mg, 0.53 mmol) in 1,4-dioxane (500 μl). The mixture was stirred for 2 hours then lithium hydroxide monohydrate (26 mg, 0.61 mmol) was added and stirring continued for 24 hours. The majority of solvents were removed by distillation in vacuo then the residue was dissolved in water (5 ml) and acidified using hydrochloric acid (1M) to pH=1. The product was extracted into dichloromethane (5×5 ml), dried (Na2SO4) and the solvent removed in vacuo to obtain (2R) 2-isobutylsuccinic acid (49 mg, 53%) as a solid. HPLC-MS (single UV peak with Rt=6.223 mins, 197.1 [M+Na]+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07132449B2 |
| 出典データセット | uspto-grants-2006_11 |
| ORD ID | ord-749d8be403974c45919568efe5ee098c |
| 出典メモ | uspto-grants-2006_11 |