3,6-Dichloropyridazine → 6-Chloro-N-methylpyridazin-3-amine

3,6-Dichloropyridazine (107, 500 mg, 3.36 mmol) was slowly added to a 2.0 M methylamine methanol solution (NH2Me in MeOH, 5 mL, 10 mmol) and stirred at room temperature for 24 hours. Water was added to the reaction mixture, and organic compounds were extracted with ethyl acetate. The recovered organic solution was washed with an aqueous solution of saturated sodium chloride and evaporated after a treatment with sodium sulfate. Purification was performed by column chromatograph to give the target compound 3-(N-monomethylamino)-6-chloropyridazine (108e, 505 mg, 88%) as a white solid.

1. extractionwere extracted with ethyl acetate
2. washThe recovered organic solution was washed with an aqueous solution of saturated sodium chloride
3. customevaporated after a treatment with sodium sulfate
4. customPurification

ORDレコード

ord-171ec25a3f954b868203a18a0508ed80

出典データセット

uspto-grants-2013_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08497260B2