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

Temperatur

70 °C

To a solution of 6-chloropyridazin-3(2H)-one (780 mg, 6 mmol) in CH3CN (40 mL) was added Cs2CO3 (3.9 g, 12 mmol) and CH3I (1 mL, 12 mmol) and the reaction mixture was stirred at 70° C. overnight. Solid was removed by filtration and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel chromatography (hexane/EA=3/1) to afford the title compound as orange oil (6.5 g, 75%). [LCMS: Rt=1.43 min, m/z 145.1 (M+H)+].

1. customSolid was removed by filtration
2. concentrationthe filtrate was concentrated under reduced pressure
3. customThe residue was purified by silica gel chromatography (hexane/EA=3/1)

ORD-Eintrag

ord-4cde32e579f84b50bd9c9ae9491f3fb4

Quelldatensatz

uspto-grants-2015_05

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09034874B2