関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Hexane | HCID 8058 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | (3-Fluorophenyl)carbamic acid benzyl ester | HCID 895321 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 生成物 | (R)-3-(3-Fluorophenyl)-5-(hydroxymethyl)oxazolidin-2-one | HCID 11229590 | 70% |
反応手順
132 g of N-carbobenzyloxy-3-fluoroaniline 132 g prepared in the Preparation example 1 was dissolved in 1.3 L of tetrahydrofuran and the solution was cooled to −78° C. 370 ml of n-buthyllitium (n-BuLi, 1.6M/n-hexane) was slowly added to the solution in a nitrogen atmosphere, followed by stirring for 10 min. And 84 ml of (R)-(−)-glycidylbuthylate was slowly added to the reaction mixture, stirred at the same temperature for 2 hours and allowed to react for 24 hours at room temperature. After completion of the reaction, the solution was added with ammonium chloride (NH4Cl) solution and extracted with 0.5 L of ethyl acetate at room temperature. The organic layer, thus separated, was washed with brine, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was dissolved in 100 ml of ethyl acetate and washed with n-hexane to give white crystals, which were purified to the title compound. 80 g. Yield 70%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07816379B2 |
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| 出典データセット | uspto-grants-2010_10 |
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| ORD ID | ord-546f43c76191422e88531931cfd1686a |
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| 出典メモ | uspto-grants-2010_10 |
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