참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | 2-Methoxy-5-methylphenol | HCID 14519 | — |
| 반응물 | 3,6-Dichloropyridazine 1-oxide | HCID 260910 | — |
| 반응물 | Potassium tert-butoxide | HCID 23665647 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 6-Chloro-3-(2-methoxy-5-methylphenoxy)pyridazine 1-oxide | HCID 22940016 | 70.2% |
반응 단계
In a mixed solvent of 1,4-dioxane (3 mL) and dimethylsulfoxide (3 mL) was dissolved 167.5 mg (1.21 mmol) of commercially available 2-methoxy-5-methylphenol, and 142.8 mg (1.27 mmol) of potassium tert-butoxide was added to the solution, then 202.9 mg (1.23 mmol) of 3,6-dichloropyridazine 1-oxide was added to the mixture and the resulting mixture was stirred at room temperature overnight. The reaction mixture was poured into water, and extracted with ethyl acetate. The organic layer was successively washed with water and brine, and dried over anhydrous magnesium sulfate. The solvent was distilled off and the obtained residue was purified by preparative thin-layer chromatography (available from MERCK CO., 1.05744, 3 plates were used, developed by ethyl acetate:hexane=2:1) to obtain 226.5 mg (0.849 mmol, Yield: 70.2%) of 6-chloro-3-(2-methoxy-5-methylphenoxy)pyridazine 1-oxide.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07964531B2 |
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| 출처 데이터셋 | uspto-grants-2011_06 |
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| ORD ID | ord-40362655c2a14723ad6a57f03b38de65 |
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| 출처 메모 | uspto-grants-2011_06 |
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