Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Water | HCID 962 | — |
| Edukt | m-Chloroperbenzoic acid | HCID 70297 | — |
| Edukt | 3-Chloro-6-(methylthio)pyridazine | HCID 252475 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 3-Chloro-6-(methylsulfonyl)pyridazine | HCID 252476 | 71% |
Reaktionsschritte
3-Chloro-6-(methylthio)pyridazine (90 mg, 0.50 mmol) synthesized in Example (118b) was dissolved in methylene chloride (10 mL), and m-chloroperbenzoic acid (220 mg, 1.00 mmol) was added, followed by stirring at 0° C. for 30 minutes under nitrogen atmosphere. Water (20 mL) was added to the reaction solution, and extraction was carried out twice with methylene chloride (10 mL). The organic layer was washed with saturated brine, and subsequently dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the resulting residue was purified using silica gel column chromatography (elution solvent: ethyl acetate/hexane=10%-100%) to afford the desired compound (77 mg, yield 71%) as a white solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08017610B2 |
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| Quelldatensatz | uspto-grants-2011_09 |
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| ORD ID | ord-fbe7481ac3fd405184b10c8372aa077d |
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| Quellennotiz | uspto-grants-2011_09 |
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