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p-Toluenesulfonic acid → Ethyl 3-oxo-(2,3,4,5-tetrafluorophenyl)propanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | 1,3-Diethyl 2-(2,3,4,5-tetrafluorobenzoyl)propanedioate | HCID 13564973 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Ethyl 3-oxo-(2,3,4,5-tetrafluorophenyl)propanoate | HCID 600916 | 71.6% |
反応手順
0.3 g of p-toluenesulphonic acid is added to an emulsion of 284.8 g of crude diethyl 2,3,4,5-tetrafluorobenzoyl-malonate in 300 ml of water. The mixture is heated at the boiling point for 4.5 hours, with thorough stirring, the cooled emulsion is extracted several times with methylene chloride, the combined methylene chloride solutions are washed once with saturated sodium chloride solution and dried with sodium sulphate and the solvent is distilled off in vacuo. Fractionation of the residue under a fine vacuum gives 160.2 g of ethyl 2,3,4,5-tetrafluorobenzoylacetate of boiling point 75°-96° C./0.06-0.09 mbar.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04753925 |
| 出典データセット | uspto-grants-1988_06 |
| ORD ID | ord-59b20f115b044d7f98e09f2d562d88f8 |
| 出典メモ | uspto-grants-1988_06 |