関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Glycine | HCID 750 | — |
| 反応物 | 1,4-Dioxane | HCID 31275 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Boc-Leu-OSu | HCID 11023929 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Ethyl acetate hexane | HCID 21226206 | — |
| 生成物 | (S)-2-(2-((tert-Butoxycarbonyl)amino)-4-methylpentanamido)acetic acid | HCID 7018768 | 75.7% |
反応手順
2.63 Grams of H-Gly-OH and 3.50 g of sodium hydrogen carbonate were suspended in 50 ml of water, to this supension was added, under ice-cooling condition, 50 ml of dioxane solution containing 10.0 g of Boc-Leu-OSu, and stirred for 30 minutes, then this mixture was further stirred at room temperature for 15 hours. The reaction mixture was concentrated under reduced pressure, and the residue thus obtained was extracted with ethyl acetate (70 ml). The ethyl acetate layer was washed with 1N-hydrochloric acid, and with a saturated sodium chloride aqueous solution, then was dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue thus obtained was recrystalled from ethyl acetate-n-hexane to obtain 6.65 g (yield: 75.7%) of the above-mentioned objective product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05204326 |
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| 出典データセット | uspto-grants-1993_04 |
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| ORD ID | ord-e827f6e001ba444aab7a9df216915011 |
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| 出典メモ | uspto-grants-1993_04 |
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