反应详情

A solution of N2-(6-chloropyrimidin-4-yl)pyridine-2,6-diamine (1) (0.25 g, 1.1 mmol) and aniline (2) (0.16 g, 1.7 mmol) in n-BuOH (25 mL) was heated at 120° C. for 12 h in a pressure tube. The reaction mixture was cooled, was dissolved in methanol (10 mL) and was concentrated under reduced pressure. The residue was dissolved in ethyl acetate (35 mL) and was washed successively with 10% sodium bicarbonate solution (20 mL), water (20 mL), and saturated brine (20 mL). The ethyl acetate extract was dried over Na2SO4 and was concentrated under reduced pressure to give a residue, which was triturated with diethyl ether to give (260 mg, 83%) N4-(6-aminopyridin-2-yl)-N6-phenylpyrimidine-4,6-diamine (3) as an off-white solid.

1. temperatureThe reaction mixture was cooled
2. concentrationwas concentrated under reduced pressure
3. dissolutionThe residue was dissolved in ethyl acetate (35 mL)
4. washwas washed successively with 10% sodium bicarbonate solution (20 mL), water (20 mL), and saturated brine (20 mL)
5. extractionThe ethyl acetate extract
6. dry with materialwas dried over Na2SO4
7. concentrationwas concentrated under reduced pressure
8. customto give a residue, which
9. customwas triturated with diethyl ether