関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Formic Acid | HCID 284 | — |
| 反応物 | 3-(2,4,6-Trifluoro-phenyl)-acrylic acid ethyl ester | HCID 57412779 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Ethyl 3-(2,4,6-trifluorophenyl)propanoate | HCID 53425006 | 89.2% |
反応手順
Pd/C (0.5 g, 10%, 50% water wet) was added to a solution of ethyl (2E)-3-(2,4,6-trifluorophenyl)-2-propenoate (2.0 g, 8.69 mmol) in ethyl acetate (40 mL) under an argon atmosphere, followed by TEA (2.409 mL, 17.38 mmol) and formic acid (1.666 mL, 43.4 mmol). The reaction mixture was refluxed at 90° C. under argon for 1 h. The reaction mixture was filtered through a celite pad and the filtrate was then washed with water, 5% NaHCO3 solution and brine, before being dried over Na2SO4. Solvent evaporation under reduced pressure yielded the title compound as a pale yellow oil (1.8 g, 89% yield). LCMS: 3.41 min, [M+H+]=232.9
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09174968B2 |
|---|
| 出典データセット | uspto-grants-2015_11 |
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| ORD ID | ord-6d7f6fd76ca64d2bbbae274533215244 |
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| 出典メモ | uspto-grants-2015_11 |
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