反应详情

Sodium hydride (108 mg, 60% mineral oil dispersion, 2.72 mmol) was placed in a dried flask under a nitrogen atmosphere, followed by sequential addition of anhydrous tetrahydrofuran (10 ml) and 2-(4-methylpiperazin-1-yl)pyridin-4-ylamine (62 mg, 0.32 mmol) with a syringe. After the resulting mixture was stirred at room temperature for 2 hours, 4-[4-chloro-5-(2-chloroethyl)-6-(3-methoxyphenyl)-pyrimidin-2-yl]morpholine (100 mg, 0.27 mmol) was added, followed by heating to reflux for 4 hours. The reaction mixture was cooled, which was subsequently added dropwise slowly onto ice water, followed by extraction twice with ethyl acetate (10 ml). The organic layer was washed with brine (10 ml), and dried over sodium sulfate, followed by distilling off under reduced pressure, to obtain a crude product as a red oil (206 mg).

1. temperatureby heating
2. temperatureto reflux for 4 hours
3. temperatureThe reaction mixture was cooled
4. additionwhich was subsequently added dropwise slowly onto ice water
5. extractionfollowed by extraction twice with ethyl acetate (10 ml)
6. washThe organic layer was washed with brine (10 ml)
7. dry with materialdried over sodium sulfate
8. distillationby distilling off under reduced pressure