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4-((4-Fluorophenyl)methylene)-2-methyl-5(4H)-oxazolone → 3,4,4-Trifluorobut-3-enyl 3-(4-fluorophenyl)-2-acetylamino-prop-2-enoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-((4-Fluorophenyl)methylene)-2-methyl-5(4H)-oxazolone | HCID 367073 | — |
| 反応物 | 3,4,4-Trifluorobut-3-en-1-ol | HCID 11768573 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 3,4,4-Trifluorobut-3-enyl 3-(4-fluorophenyl)-2-acetylamino-prop-2-enoate | HCID 54179696 | 49.1% |
反応手順
8.2 g (40 mmol) of 2-methyl-4-(4-fluorobenzylidene)-oxazol-5-one of Example (II-1) in 100 ml of toluene are heated overnight under reflux with 6.3 g (50 mmol) of 3,4,4-trifluorobut-3-enol, with the addition of 200 mg of 4-dimethylaminopyridine. After cooling, the solution is washed with water and concentrated under reduced pressure and the brown solid is chromatographed over silica gel using the system chloroform/ethyl acetate (4:1). 6.5 g (Yield 49% of theory) of 3,4,4-trifluorobut-3-enyl 3-(4-fluorophenyl)-2-acetylamino-prop-2-enoate of mp.: 116° are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06004992 |
| 出典データセット | uspto-grants-1999_12 |
| ORD ID | ord-c1ef2b91c0084b979560fcc2f9fcf530 |
| 出典メモ | uspto-grants-1999_12 |