関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Chloroform | HCID 6212 | — |
| 反応物 | Benzyloxycarbonyl-L-proline | HCID 101987 | — |
| 反応物 | L-Leucine, ethyl ester, hydrochloride (1:1) | HCID 11658447 | — |
| 反応物 | Ethyl cyano{[(methanesulfonyl)oxy]imino}acetate | HCID 54531055 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | Ethyl N-(1-((benzyloxy)carbonyl)-L-prolyl)-L-leucinate | HCID 6453075 | 40.9% |
反応手順
N-Benzyloxycarbonyl-L-proline (1.25 g) and L-leucine ethyl ester hydrochloride (1.0 g) are suspended into chloroform (10 ml), and therein is dissolved triethylamine (1.40 ml). To the solution is added ethyl 2-methanesulfonyloxyimino-2-cyanoacetate (1.1 g) and the mixture is stirred at room temperature for 16 hours. After reaction, the reaction mixture is extracted with ethyl acetate. The extract is washed with water, 1 N aqueous sodium hydrogen carbonate, water, 1 N hydrochloric acid and water in order and then dried over anhydrous magnesium sulfate. After drying, the solvent is distilled off and the resulting residue is crystallized from petroleum ether to give N-(N-benzyloxycarbonyl-L-prolyl)-L-leucine ethyl ester (0.8 g), melting point: 65°-67° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04242507 |
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| 出典データセット | uspto-grants-1980_12 |
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| ORD ID | ord-8efbbd2f237244b7b894d13b45c3f98b |
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| 出典メモ | uspto-grants-1980_12 |
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