化工社化工社 化学情報印刷レポート · 研究参考用
Methyl Acrylate → Methyl 4-cyano-4-(2-trifluoromethylphenyl)butanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl Acrylate | HCID 7294 | — |
| 反応物 | 18-Crown-6 | HCID 28557 | — |
| 反応物 | 2-(Trifluoromethyl)phenylacetonitrile | HCID 76435 | — |
| 触媒 | Potassium tert-butoxide | HCID 23665647 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Methyl 4-cyano-4-(2-trifluoromethylphenyl)butanoate | HCID 66618793 | — |
反応手順
2-(Trifluoromethyl)phenylacetonitrile (2.0 g) was dissolved in tetrahydrofuran (50 mL). Potassium tert-butoxide (60.6 mg), 18-crown-6 (2.85 g) and methyl acrylate (973 μL) were added at 0° C. and the mixture was stirred at the same temperature for 40 minutes. The reaction was terminated with saturated ammonium chloride, followed by dilution with ethyl acetate. The organic layer was washed with brine and dried over magnesium sulfate. Concentration under reduced pressure gave an oil. The oil was purified by silica gel column chromatography (mobile phase:ethyl acetate/heptane=0 to 30%) to obtain the title compound (2.2 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08754100B2 |
| 出典データセット | uspto-grants-2014_06 |
| ORD ID | ord-af00e3dc846f42daacbf0b123124741a |
| 出典メモ | uspto-grants-2014_06 |