Potassium Carbonate → HCID 66864935, compound

Temperature

55 °C

To a suspension of 4.00 g (24.2 mmol) of 4,5-dichloro-2H-pyridazin-3-one and 6.70 g (48.5 mmol) of potassium carbonate in 40 ml of acetone were added 4.55 ml (6.74 g, 48.5 mmol, 2 eq.) of 2-bromoethylmethylether. The suspension was stirred for 24 h at 55° C. Then 1 ml (1.48 g, 10.6 mmol) of 2-bromoethylmethylether were added and the mixture was stirred for another 24 h. The reaction was then allowed to cool to room temperature, the solids were filtered off and washed twice with ethyl acetate. The filtrate was concentrated in vaccuo, taken up in methylene chloride and purified by flash chromatography (SiO2, heptane:ethyl acetate 85:15 v/v) to yield the title compound as a white crystalline solid.

1. stirringthe mixture was stirred for another 24 h
2. temperatureto cool to room temperature
3. filtrationthe solids were filtered off
4. washwashed twice with ethyl acetate
5. concentrationThe filtrate was concentrated in vaccuo
6. custompurified by flash chromatography (SiO2, heptane:ethyl acetate 85:15 v/v)

ORD record

ord-1c38dd633a8d490191f715478f25a946

Source dataset

uspto-grants-2012_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08334287B2