反应详情

温度

145 °C

To a solution of N2-(6-chloropyrimidin-4-yl)pyridine-2,6-diamine (100 mg, 0.45 mmol) in DMF (1 mL) was added 3-methylphenol (88 mg, 0.8 mmol) and anhydrous K2CO3 (93 mg, 0.6 mmol). The reaction mixture was heated at 145° C. for 16 h. It was then cooled and DMF was removed under reduced pressure to get a yellow gummy residue. The residue was taken in EtOAc (20 mL) and washed with water (5 mL), brine (5 mL) and dried over Na2SO4. Filtration followed by concentration under reduced pressure afforded a yellow gum which was further purified by column chromatography (SiO2, 60-120, EtOAc/hexane, 5/5) to give N2-(6-(3-methylphenoxy)pyrimidin-4-yl)pyridine-2,6-diamine (IR-12) (100 mg, 75%) as a pale yellow solid.

1. temperatureIt was then cooled
2. customDMF was removed under reduced pressure
3. customto get a yellow gummy residue
4. washwashed with water (5 mL), brine (5 mL)
5. dry with materialdried over Na2SO4
6. filtrationFiltration
7. concentrationfollowed by concentration under reduced pressure
8. customafforded a yellow gum which
9. customwas further purified by column chromatography (SiO2, 60-120, EtOAc/hexane, 5/5)