関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | L-Phenylalanine | HCID 6140 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Carbonate Ion | HCID 19660 | — |
| 反応物 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | Fmoc-phenylalanine | HCID 978331 | 75% |
反応手順
0.83 g of L-phenylalanine (5 mmoles) are dissolved in aqueous dioxan (1: 2, 12 ml) containing 1.4 ml of triethylamine (10 mmoles). The mixture is cooled to 0° C. and 2.05 g (5 mmoles of the preceding carbonate dissolved in 4 ml of dioxan added at one time. After two hours at 0° C., 20 ml of water are added, followed by extraction twice with 20 ml of ether. The aqueous phase is then acidified (pH 2-3) with 6 N HCl followed by extraction three times with 50 ml of ethyl acetate. This is followed by drying over MgSO4 and evaporation. The product obtained crystallizes from ethyl acetate and petroleum-ether, and 1.44 g of the desired derivative obtained (yield 75%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04960881 |
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| 出典データセット | uspto-grants-1990_10 |
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| ORD ID | ord-ed3c8d975fb94393be521c0025c9887f |
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| 出典メモ | uspto-grants-1990_10 |
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