Methyl iodide → 6-Chloro-2-methyl-2,3-dihydropyridazin-3-one

To a solution 6-chloropyridazin-3(2H)-one (130 mg, 1.0 mmol) in acetonitrile (3.0 mL) was added K2CO3 (437 mg, 3.16 mmol), CH3I (299 mg, 2.11 mmol), the reaction mixture was stirred at reflux for 2 h. The mixture was cooled to ambient temperature, diluted with EtOAc (20 mL), washed with sodium bicarbonate (10 mL) and brine (10 mL), dried over MgSO4, filtered and concentrated. The residue was purified with silica gel column (Petroleum ether:ethyl acetate=4:1) to obtained product: LC/MS m/z=145 (M+H)+.

1. temperatureat reflux for 2 h
2. washwashed with sodium bicarbonate (10 mL) and brine (10 mL)
3. dry with materialdried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue was purified with silica gel column (Petroleum ether:ethyl acetate=4:1)
7. customto obtained product

ORD-Eintrag

ord-8a9f4b1f7eea4bc698fd87d0c961aa8d

Quelldatensatz

uspto-grants-2016_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09273033B2