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HRID 429256作成日:2026年10月25日
Dimethylamine → 5-Amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-3-(N,N-dimethylamidino)-4-trifluoromethylsulfinylpyrazole
https://huagongshe.com/reaction/429256
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylamine | HCID 674 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Fipronil | HCID 3352 | — |
| 反応物 | Sodium Chloride | HCID 5234 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 5-Amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-3-(N,N-dimethylamidino)-4-trifluoromethylsulfinylpyrazole | HCID 18354775 | 27% |
反応手順
5-Amino-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-trifluoromethylsulfinylpyrazole (0.97 g, 2.22 mmol) was dissolved in 10 ml of 1,4-dioxane and dimethylamine (50% aqueous solution) (1.20 ml, 11.4 mmol) was added, and then the mixture was stirred at room temperature for 5 days. After stirring, 20 ml of water and 20 ml of an aqueous saturated sodium chloride solution were added and the solution was extracted twice with 30 ml of ethyl acetate. The extract was dried over anhydrous magnesium sulfate and the solvent was distilled off to obtain a yellow amorphous. The amorphous was subjected to silica gel column chromatography [eluent: mixed solvent of ethyl acetate and methanol (volume ratio=4:1)] and a small amount of ether was added to crystallize the resulting amorphous. This resultant was filtered to obtain 0.29 g (0.60 mmol) of the title compound as a colorless crystal. Yield 27%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06316477B1 |
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| 出典データセット | uspto-grants-2001_11 |
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| ORD ID | ord-0dfb01ce0f7c426f8def0d1255659a48 |
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| 出典メモ | uspto-grants-2001_11 |
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