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Dichloroacetyl chloride → 5-Dichloroacetamido-1-(2,3,6-trichloro-4-trifluoromethyl-phenyl)-pyrazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dichloroacetyl chloride | HCID 6593 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 1H-Pyrazol-5-amine, 1-[2,3,6-trichloro-4-(trifluoromethyl)phenyl]- | HCID 13689613 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 5-Dichloroacetamido-1-(2,3,6-trichloro-4-trifluoromethyl-phenyl)-pyrazole | HCID 13913430 | 93.5% |
反応手順
15.3 g (0.145 mol) of anhydrous sodium carbonate and 4.76 ml (0.048 mol) of 98% strength dichloroacetyl chloride are added in succession, at 5° C. to 10° C., to 8.0 g (0.024 mol) of 5-amino-1-(2,3,6-trichloro-4-trifluoromethyl-phenyl)-pyrazole in 80 ml of dichloromethane. The mixture is stirred for 4 hours at 5° C.-10° C. and for 13 hours at room temperature. The mixture is diluted with 80 ml of dichloromethane, filtered, and washed in succession with water and saturated sodium chloride solution. The organic phase is dried over magnesium sulphate and freed from the solvent in vacuo. 10.0 g (93.5% of theory) of 5-dichloroacetamido-1-(2,3,6-trichloro-4-trifluoromethyl-phenyl)-pyrazole of melting point 156° C.-161° C. are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04764202 |
| 出典データセット | uspto-grants-1988_08 |
| ORD ID | ord-c3d814524d1c47dabe278a17cca85bd0 |
| 出典メモ | uspto-grants-1988_08 |