تفاعل #491973

معادلة التفاعل

2-methylamino-6-aminopyridine

4,6-dichloropyrimidine

DIPEA

→

N2-(6-chloropyrimidin-4-yl)-N6-methylpyridine-2,6,diamine

المردود 33.0%

المذيبات

n-butanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe reaction mixture was cooled
2. 2
   تركيزwas concentrated under reduced pressure
3. 3
   غسيلThe dichloromethane solution was washed with NaHCO3 solution (2 mL), water (2 mL) and brine (2 mL)
4. 4
   تجفيفwas dried over Na2SO4
5. 5
   تركيزwas concentrated under reduced pressure
6. 6
   أخرىThe residue was purified by column chromatography (SiO2, 60-120, petroleum ether/ethyl acetate, 6/4)

الإجراء التجريبي

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.

المصدر