4,6-Dichloropyrimidine → n2-(6-Chloropyrimidin-4-yl)-n6-methylpyridine-2,6,diamine

A mixture of 2-methylamino-6-aminopyridine (0.5 g, 4.04 mmol), 4,6-dichloropyrimidine (1.51 g, 10.13 mmol), DIPEA (1.5 g, 12.17 mmol) in n-butanol (5 mL) was heated at 120° C. for 16 h. The reaction mixture was cooled, was concentrated under reduced pressure and the residue was taken in dichloromethane (25 mL). The dichloromethane solution was washed with NaHCO3 solution (2 mL), water (2 mL) and brine (2 mL), was dried over Na2SO4 and was concentrated under reduced pressure. The residue was purified by column chromatography (SiO2, 60-120, petroleum ether/ethyl acetate, 6/4) to give N2-(6-chloropyrimidin-4-yl)-N6-methylpyridine-2,6,diamine (0.3 g, 33%) as a yellow solid.

1. temperatureThe reaction mixture was cooled
2. concentrationwas concentrated under reduced pressure
3. washThe dichloromethane solution was washed with NaHCO3 solution (2 mL), water (2 mL) and brine (2 mL)
4. dry with materialwas dried over Na2SO4
5. concentrationwas concentrated under reduced pressure
6. customThe residue was purified by column chromatography (SiO2, 60-120, petroleum ether/ethyl acetate, 6/4)

ORD-Eintrag

ord-2f4105a75c8642408771e993073bd670

Quelldatensatz

uspto-grants-2016_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09296704B2