참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Fipronil | HCID 3352 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 용매 | Hexane | HCID 8058 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | HCID 136109406 | HCID 136109406 | 65.5% |
반응 단계
5-Amino-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-trifluoromethylsulfinylpyrazole (500 mg, 1.1 mmol) and hydroxylamine hydrochloride (79 mg, 1.1 mmol) were dissolved in 5 ml of dioxane, and then triethylamine (115 mg, 1.1 mmol) was added at room temperature. After the mixture was stirred at room temperature for 6 hours, hydroxylamine hydrochloride (79 mg, 1.1 mmol) and triethylamine (115 mg, 1.1 mmol) were further added, followed by stirring at room temperature for 2 hours. The reaction mixture was poured into 100 ml of iced water and extracted with 100 ml of ethyl acetate. The extract was dried over anhydrous magnesium sulfate and then concentrated to obtain a brown oily substance. This oily substance was subjected to silica gel column chromatography [eluent: mixed solvent of n-hexane and ethyl acetate (volume ratio=3:1)] to obtain 340 mg (0.72 mmol) of the title compound as a colorless crystal. Yield 63%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06316477B1 |
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| 출처 데이터셋 | uspto-grants-2001_11 |
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| ORD ID | ord-7478df3361dc4c8b894a280c733d45fc |
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| 출처 메모 | uspto-grants-2001_11 |
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