関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Itaconic acid | HCID 811 | — |
| 反応物 | Isopropanol | HCID 3776 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Methylsuccinic acid | HCID 10349 | — |
反応手順
In a 20 ml-volume Schlenk's tube were charged 65.0 mg (0.5 mmole) of itaconic acid and 14.91 mg (0.01 mmole) of [RuH((-)-BINAP)2 ]PF6, and 2.5 ml of tetrahydrofuran (THF) and 2.5 ml (32.7 mmole) of isopropyl alcohol were added thereto. The mixture was heated at reflux in an oil bath at 85° C. for 24 hours. The solvent was removed by distillation under reduced pressure. The residue was dissolved in 20 ml of a 1M sodium hydroxide aqueous solution and washed three times with each 10 ml portions of chloroform. The aqueous layer was adjusted to a pH of 1 with concentrated hydrochloric acid and then extracted three times with each 10 ml portions of diethyl ether. The combined ether layer was dried over magnesium sulfate, and the solvent was removed to give 47 to 60 mg of methylsuccinic acid as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05334758 |
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| 出典データセット | uspto-grants-1994_08 |
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| ORD ID | ord-2f120d45741c4147aafff66717a49808 |
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| 出典メモ | uspto-grants-1994_08 |
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