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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

反応式

関与物質

役割名称HCID仕込み量
反応物DimethylamineHCID 674—
反応物WaterHCID 962—
反応物FipronilHCID 3352—
反応物Sodium ChlorideHCID 5234—
溶媒MethanolHCID 887—
溶媒Diethyl EtherHCID 3283—
溶媒Ethyl AcetateHCID 8857—
溶媒1,4-DioxaneHCID 31275—
生成物5-Amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-3-(N,N-dimethylamidino)-4-trifluoromethylsulfinylpyrazoleHCID 1835477527%

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

DOI10.6084/m9.figshare.5104873.v1
特許番号US06316477B1
出典データセットuspto-grants-2001_11
ORD IDord-0dfb01ce0f7c426f8def0d1255659a48
出典メモuspto-grants-2001_11