Hydrochloric Acid → HCID 71306242, compound

2,4-Dichloro-5-methoxypyrimidine (10 g) was dissolved in THF (100 ml), and while cooling, iron(III) acetylacetone (1.97 g), methyl magnesium chloride (3.0 M: 22.4 ml) were then added to the solution. The obtained mixture was stirred at room temperature overnight. Thereafter, iron(III) acetylacetone (1.97 g), and methyl magnesium chloride (3.0 M: 22.4 ml) were added to the reaction solution further twice. Thereafter, a 1 N hydrochloric acid aqueous solution was added to the reaction mixture, and diethyl ether was then added to the reaction solution to carry out liquid separation and extraction. 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 (6.6 g).

1. temperaturewhile cooling
2. additionwas then added to the reaction solution
3. customliquid separation and extraction
4. dry with materialThe organic layer was dried over magnesium sulfate
5. concentrationthe solvent was then concentrated under reduced pressure
6. customThe obtained residue was purified by silica gel column chromatography (n-heptane:ethyl acetate)

ORD record

ord-5108f3e85a6e476ea96bec4af2148b9c

Source dataset

uspto-grants-2012_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08268848B2