Water → 3-Chloro-6-(methylsulfonyl)pyridazine

温度

0 °C

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.

1. washThe organic layer was washed with saturated brine
2. dry with materialsubsequently dried over anhydrous magnesium sulfate
3. distillationThe solvent was distilled off under reduced pressure
4. customthe resulting residue was purified
5. washsilica gel column chromatography (elution solvent: ethyl acetate/hexane=10%-100%)

ORDレコード

ord-fbe7481ac3fd405184b10c8372aa077d

出典データセット

uspto-grants-2011_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08017610B2