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Dicyclohexylcarbodiimide → N-(3-methoxycarbonyl-2-methylpropanoyl)-L-alanine benzyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dicyclohexylcarbodiimide | HCID 10868 | — |
| 反応物 | 4-Methyl hydrogen 2-methylenesuccinate | HCID 81791 | — |
| 反応物 | benzyl (2S)-2-aminopropanoate | HCID 726858 | — |
| 反応物 | 4-Methoxy-2-methyl-4-oxobutanoic acid | HCID 4563901 | — |
| 反応物 | HCID 178418300 | HCID 178418300 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | N-(3-methoxycarbonyl-2-methylpropanoyl)-L-alanine benzyl ester | HCID 53826083 | — |
反応手順
L-alanine benzyl ester (44.7 g.) and hydroxybenzotriazole (34 g.) are dissolved in dioxane (750 ml.) and the solution is chilled with stirring in an ice-water bath. Dicyclohexylcarbodiimide (51.5 g.) and 3-methoxycarbonyl-2-methylpropanoic acid (36 g.), prepared by hydrogenation of 3-methoxycarbonyl-2-methylene propanoic acid, are added in that order and the mixture is stirred at room temperature for 18 hours. The precipitate is filtered off, and the filtrate is concentrated to dryness in vacuo. The residue is dissolved in ethyl acetate and washed neutral. The ethyl acetate is dried over magnesium sulfate and concentrated to dryness in vacuo to yield N-(3-methoxycarbonyl-2-methylpropanoyl)-L-alanine benzyl ester.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04146639 |
| 出典データセット | uspto-grants-1979_03 |
| ORD ID | ord-01a02a29d308472eb399c818f8e8993f |
| 出典メモ | uspto-grants-1979_03 |