関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | methyl (2S)-2-[ethyl-(4-fluorophenyl)sulfonyl-amino]-3-hydroxy-propanoate | HCID 131736579 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 2-[Ethyl-(4-fluorophenyl)sulfonyl-amino]prop-2-enoic acid | HCID 90384201 | 71.2% |
反応手順
A solution of 3B (1.1 g, 3.6 mmol) in dioxane (25 mL) was added with 20% NaOH aq. solution (20 mL) and the mixture heated at 80° C. for 4 h. The organic solvent was removed under reduced pressure and the aqueous phase acidified with 10% HCl and extracted with CH2Cl2 (3×30 mL). The combined organic phases were dried using Na2SO4, evaporated under reduced pressure and then the resulting residue purified by flash chromatography (100% EtOAc) to obtain 4B as white solid (0.7 g, 66% yield). 1HNMR (DMSO, 200 MHz) δ 1.12 (t, 3H), 3.29 (q, 2H), 5.69 (s, 1H), 6.32 (s, 1H), 7.39 (m, 2H), 7.89 (m, 2H), 12.9 (bs, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09409864B2 |
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| 出典データセット | uspto-grants-2016_08 |
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| ORD ID | ord-292ee0f14b2147f98b8b4574d6453987 |
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| 出典メモ | uspto-grants-2016_08 |
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