関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Ethyl 1-ethyl-5-oxoprolinate | HCID 15225833 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | L-Proline, 1-ethyl-5-oxo- | HCID 18605196 | 99.3% |
反応手順
Ethyl 1-ethyl-5-oxoprolinate (1.33 g, 7.18 mmol) was dissolved in ethanol (10 ml) and cooled to 0° C. in an ice bath. To this was added 12.5M aqueous sodium hydroxide solution (1.72 ml, 21.53 mmol) and the mixture was stirred for ˜4 hours at 0° C. The ethanol was evaporated under vacuum and the aqueous residue was acidified with 2N aqueous hydrogen chloride to pH1. The volume of the aqueous phase was reduced to ˜3 ml under vacuum and then extracted with a 3:1 mixture of chloroform and isopropanol using a phase separator. The combined organic layers were concentrated to a pale yellow oil which on drying in vacuo crystallized to give 1-ethyl-5-oxoproline as a white solid (1.12 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07718693B2 |
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| 出典データセット | uspto-grants-2010_05 |
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| ORD ID | ord-c7717be610cf4281a79b5b51e39f4c4b |
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| 出典メモ | uspto-grants-2010_05 |
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