Chloroform → 5-Methoxy-2,4-dimethylpyrimidine

Temperatur

75 °C

2,4-Dichloro-5-methoxypyrimidine (5.3 g) was dissolved in THF (51.3 ml), and tetrakis(triphenylphosphine)palladium (1.71 g) and trimethylaluminum (2.0 M: 51.8 ml) were then added to the solution. The temperature of the obtained mixture was heated to 75° C., and the obtained mixture was then stirred overnight. Thereafter, 1 equivalent of trimethyl aluminum was added to the reaction solution, and the obtained mixture was then stirred for 6 hours. Thereafter, saturated ammonium chloride aqueous solution was added dropwise to the reaction solution under cooling on ice, and liquid separation and extraction were carried out with chloroform. 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 to ethyl acetate), so as to obtain the title compound (4.2 g).

1. stirringthe obtained mixture was then stirred for 6 hours
2. temperatureunder cooling on ice, and liquid separation and extraction
3. dry with materialThe organic layer was dried over magnesium sulfate
4. concentrationthe solvent was then concentrated under reduced pressure
5. customThe obtained residue was purified by silica gel column chromatography (n-heptane:ethyl acetate to ethyl acetate)

ORD-Eintrag

ord-453f65ddecc94a53814caff9aa8883c3

Quelldatensatz

uspto-grants-2012_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08268848B2