反应详情

To a solution of (3-chloro-phenyl)-[4-(2-chloro-pyridin-4-yl)-pyrimidin-2-yl]-amine (4.8 g, 0.015 mol) in pyrrolidon (20 ml) is added sodium hydride (1.93 g, 0.06 mmol of a 75% dispersion in oil) in several portions. The reaction temperature is slowly raised to +150° C. After 30 minutes the heating bath is removed and the mixture is poured onto crushed ice. The reaction mixture is partitioned between ethyl acetate and water. The organic phase is separated, dried over magnesium sulfate, filtered and evaporated under reduced presssure. The residue is purified by silicagel chromatography and recrystallized from ethyl acetate to give the title compound, m.p. 165–166° C.

1. temperatureThe reaction temperature is slowly raised to +150° C
2. customAfter 30 minutes the heating bath is removed
3. additionthe mixture is poured
4. customonto crushed ice
5. customThe reaction mixture is partitioned between ethyl acetate and water
6. customThe organic phase is separated
7. dry with materialdried over magnesium sulfate
8. filtrationfiltered
9. customevaporated under reduced presssure
10. customThe residue is purified by silicagel chromatography
11. customrecrystallized from ethyl acetate