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Diethyl (2,4-dichloro-3,6-difluorobenzoyl)-malonate → Ethyl (2,4-dichloro-3,6-difluorobenzoyl)acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethyl (2,4-dichloro-3,6-difluorobenzoyl)-malonate | HCID 15070034 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Ethyl (2,4-dichloro-3,6-difluorobenzoyl)acetate | HCID 15070035 | 49.8% |
反応手順
0.04 g of p-toluenetoluenesulphonic acid is added to an emulsion of 34.7 g of crude diethyl (2,4-dichloro-3,6-difluorobenzoyl)-malonate in 40 ml of water. The mixture is heated at the boiling point for 3 hours, while stirring thoroughly, the cooled emulsion is extracted several times with methylene chloride, the combined CH2Cl2 solutions are washed once with saturated sodium chloride solution and dried with Na2SO4 and the solvent is distilled off in vacuo. Fractionation of the residue (33.9 g) in vacuo gives 13.9 g of ethyl (2,4-dichloro-3,6-difluorobenzoyl)-acetate of boiling point 110°-115° C./0.05 mbar, nD25 : 1,5241.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05416096 |
| 出典データセット | uspto-grants-1995_05 |
| ORD ID | ord-85d2a1a297be4b2a927b6c639d4588a1 |
| 出典メモ | uspto-grants-1995_05 |