関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | (2,4-Dichlorophenoxy)acetyl chloride | HCID 69887 | — |
| 反応物 | 5-Amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-pyrazole | HCID 13557109 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 5-(2,4-Dichlorophenoxyacetamido)-1-(2,6-dichloro-4-trifluoromethylphenyl)-pyrazole | HCID 13911739 | 94.3% |
反応手順
2.2 ml (0.0275 mol) of anhydrous pyridine and 6.7 g (0.027 mol) of 96.3 percent strength 2,4-dichlorophenoxyacetyl chloride are added successively to 8 g (0.027 mol) of 5-amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-pyrazole (cf. U.S. Pat. No. 4,614,533, supra, in 60 ml of dichloromethane with stirring at 0° C. to 5° C. and the mixture is stirred for 16 hours at room temperature. The mixture is worked up by adding 100 ml of dichloromethane, washing successively with dilute hydrochloric acid, saturated sodium bicarbonate solution and saturated sodium chloride solution, drying the organic phase over magnesium sulphate and removing the solvent in vacuo. 12.7 g (94.3% of theory) of 5-(2,4-dichlorophenoxyacetamido)-1-(2,6-dichloro-4-trifluoromethylphenyl)-pyrazole of melting point 167° C.-180° C. are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04734125 |
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| 出典データセット | uspto-grants-1988_03 |
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| ORD ID | ord-55b6c277f7e24b56919f2ba491507085 |
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| 出典メモ | uspto-grants-1988_03 |
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