참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 2,6-Dimethylphenol | HCID 11335 | — |
| 반응물 | 1,4-Dioxane | HCID 31275 | — |
| 반응물 | 3,6-Dichloropyridazine 1-oxide | HCID 260910 | — |
| 반응물 | Potassium tert-butoxide | HCID 23665647 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 생성물 | 6-Chloro-3-(2,6-dimethylphenoxy)pyridazine 1-oxide | HCID 23013801 | 63.2% |
반응 단계
268 mg (2.20 mmol) of 2,6-dimethylphenol, 1,4-dioxane (3 mL) and dimethylsulfoxide (3 mL) were mixed, 270 mg (2.41 mmol) of potassium tert-butoxide was added to the mixture in an ice bath, and the resulting mixture was stirred for 10 minutes. To the mixture was added 370 mg (2.24 mmol) of 3,6-dichloropyridazine 1-oxide, and the resulting mixture was stirred at room temperature for 10 hours and allowed to stand for 2 days. The reaction mixture was poured into ice-cold water, and extracted with ethyl acetate. The organic layers were combined, washed successively with water and brine, and dried over anhydrous sodium sulfate. The solvent was removed, and the residue was purified by silica gel column chromatography (hexane: ethyl acetate, gradient) to obtain 350 mg (1.39 mmol, Yield: 63.1%) of 6-chloro-3-(2,6-dimethylphenoxy)pyridazine 1-oxide.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07608563B2 |
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| 출처 데이터셋 | uspto-grants-2009_10 |
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| ORD ID | ord-fb9040a4c4904a93b5f198518a099289 |
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| 출처 메모 | uspto-grants-2009_10 |
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