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Dicyclohexylcarbodiimide → N-(3-acetylthio-2-trifluoromethylpropanoyl)-L-proline tertbutyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dicyclohexylcarbodiimide | HCID 10868 | — |
| 反応物 | L-Proline 1,1-dimethylethyl ester | HCID 6453108 | — |
| 反応物 | 3-Acetylthio-2-trifluoromethylpropanoic acid | HCID 12833014 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-(3-acetylthio-2-trifluoromethylpropanoyl)-L-proline tertbutyl ester | HCID 54253056 | — |
反応手順
L-proline tert-butyl ester (5.1 g.) is dissolved in dichloromethane (40 ml.) and the solution is stirred and chilled in an ice bath. Dicyclohexylcarbodiimide (6.2 g.) dissolved in dichloromethane (15 ml.) is added followed immediately by a solution of 3-acetylthio-2-trifluoromethylpropanoic acid (6.5 g.) in dichloromethane (5 ml.). After fifteen minutes stirring in the ice bath and sixteen hours at room temperature, the precipitate formed is filtered off and the filtrate is concentrated to dryness in vacuo. The residue is dissolved in ethyl acetate and washed neutral. The organic phase is dried over magnesium sulfate and concentrated to dyrness in vacuo to give N-(3-acetylthio-2-trifluoromethylpropanoyl)-L-proline tert-butyl ester.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04734420 |
| 出典データセット | uspto-grants-1988_03 |
| ORD ID | ord-4665f1d8119d40ddb020ae3e8d9c3a1f |
| 出典メモ | uspto-grants-1988_03 |