참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Sulfite | HCID 24437 | — |
| 반응물 | m-Chloroperbenzoic acid | HCID 70297 | — |
| 반응물 | 6-Chloro-3-[2-(methylsulfanyl)phenoxy]pyridazine 1-oxide | HCID 22939933 | — |
| 용매 | 1,2-Dichloroethane | HCID 11 | — |
| 생성물 | 6-Chloro-3-[2-(methylsulfonyl)phenoxy]pyridazine 1-oxide | HCID 22940050 | 56.7% |
반응 단계
In 1,2-dichloroethane (5 mL) was dissolved 208 mg (0.774 mmol) of 6-chloro-3-[2-(methylsulfanyl)phenoxy]pyridazine 1-oxide obtained in Example 11 (1), 829 mg (3.84 mmol) of 80% m-chloroperbenzoic acid was added to the solution and the resulting mixture was stirred at room temperature for 4 hours. The reaction mixture was poured into 10% aqueous sodium sulfite solution, and extracted with ethyl acetate. The organic layers were combined, washed with 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, developed by hexane:ethyl acetate=1:1) to obtain 132 mg (0.439 mmol, Yield: 56.7%) of 6-chloro-3-[2-(methylsulfonyl)phenoxy]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-c3c679b7915647d6aefb22a6a413adf1 |
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| 출처 메모 | uspto-grants-2009_10 |
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