関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Cesium fluoride | HCID 25953 | — |
| 反応物 | Diethyl 2-benzylpropanedioate | HCID 69090 | — |
| 生成物 | Ethyl 3-phenyl-2-hydroxy-2-ethoxycarbonyl-propanoate | HCID 15828909 | — |
反応手順
A mixture of diethyl benzylpropanedioate (41 g) and CsF (49.8 g) in 90 mL of DMF was heated at 40° C. with vigorous air bubbling for 3 days. The resulting mixture was diluted with ethyl acetate (800 mL) and washed with water (3×1 L). The organic layer was concentrated and then purified by Biotage silica gel column chromatography (5-20% ethyl acetate in hexanes) to give the title product as a colorless oil. 1H NMR (300 MHz, CDCl3) δ: 7.22-7.26 (m, 5H), 4.23 (q, J=7.2 Hz, 4H), 3.80 (br, 1H), 3.35 (s, 2H), 1.26 (t, J=7.2 Hz, 6H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09085568B2 |
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| 出典データセット | uspto-grants-2015_07 |
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| ORD ID | ord-7d16928b70f44c9699e03c981cf62f1d |
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| 出典メモ | uspto-grants-2015_07 |
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