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Tetrafluoroethylene → Ethyl 1-(4-ethoxyphenyl)-2,2,3,3-tetrafluorocyclobutane carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tetrafluoroethylene | HCID 8301 | — |
| 反応物 | Benzeneacetic acid, 4-ethoxy-alpha-methylene-, ethyl ester | HCID 6454764 | — |
| 触媒 | (+-)-alpha-Pinene | HCID 6654 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | Ethyl 1-(4-ethoxyphenyl)-2,2,3,3-tetrafluorocyclobutane carboxylate | HCID 13239546 | 75% |
反応手順
2-(4-ethoxyphenyl)propenoic acid ethyl ester (13.2 g) was mixed with benzene (7.5 ml), α-pinene (2 drops) N-ethyldiisopropyl amine (2 drops) and tetrafluoroethylene (15.5 ml) and heated to 150°-155° for 24 hours then 155°-160° C. for 17 hours. After evaporation of volatile materials the residue (16.6 g) was dissolved in dichloromethane and chromatographed on a column of silica gel to give the ester as a colourless oil 14.5 g (75%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04235926 |
| 出典データセット | uspto-grants-1980_11 |
| ORD ID | ord-cb3cc7b1544641ca9e96a082ef43d9ed |
| 出典メモ | uspto-grants-1980_11 |