Hydrochloric Acid → HCID 86664266, compound

2,4-Dichloro-5-methoxypyrimidine (5 g) was dissolved in THF (50 ml), and while cooling, iron(III) acetylacetone (985 mg) and ethyl magnesium chloride (0.91 M: 36.9 ml) were then added to the solution. The obtained mixture was stirred at room temperature overnight. Thereafter, iron(III) acetylacetone (985 mg) and methyl magnesium chloride (0.91 M: 36.9 ml) were added to the reaction solution further twice. A 1 N hydrochloric acid aqueous solution was added to the reaction mixture, and liquid separation and extraction were then carried out with diethyl ether. The organic layer was dried over magnesium sulfate, and the solvent was then concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (n-heptane:ethyl acetate), so as to obtain the title compound (1 g).

1. temperaturewhile cooling
2. dry with materialThe organic layer was dried over magnesium sulfate
3. concentrationthe solvent was then concentrated under reduced pressure
4. customThe obtained residue was purified by silica gel column chromatography (n-heptane:ethyl acetate)

ORD record

ord-9313fcc820c34415a7e3b7680ca82709

Source dataset

uspto-grants-2012_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08268848B2