反应详情

温度

0 °C

Under nitrogen atmosphere, 2-(6-bromo-2-methylpyrimidin-4-ylamino)thiazole-5-formic acid (Compound 12) (15.8 g, 0.05 mol), PDCP (9.0 mL, 0.06 mol) and 2-chloro-6-methylaniline (Compound 8)) (7.4 mL, 0.06 mol) were added into methylene dichloride (650 mL) by stirring and cooling, and then triethylamine (20.4 mL, 0.15 mol) was added by droplets at 0° C. When finish adding, it reacted by stirring at room temperature overnight. Saturated sodium bicarbonate aqueous solution was added and stirred for 15 mins and then filtrated. The cake was taken up and added in DMSO (80 mL) and heated to 60° C.-70° C. when stirring. After dissolving, the mixture of water and ethanol (1:1, 320 mL) was added in thermal insulation. Crystals precipitated by stirring and then cooled down to 0° C. to grow the grain for 1 h. After air pump filtration the cake was rinsed by water and then by the mixture of water and ethanol (1:1), and dried by air pump. With phosphorus pentoxide as an auxiliary desiccant, the cake was dried by vacuum (−0.095 MPa) at about 50° C. to give Compound 14 (17.0 g, yield: 77.5%).

1. temperaturecooling
2. additionWhen finish adding
3. customit reacted
4. stirringby stirring at room temperature overnight
5. stirringstirred for 15 mins
6. filtrationfiltrated
7. additionadded in DMSO (80 mL)
8. temperatureheated to 60° C.-70° C. when
9. stirringstirring
10. dissolutionAfter dissolving
11. additionthe mixture of water and ethanol (1:1, 320 mL)
12. additionwas added in thermal insulation
13. customCrystals precipitated
14. stirringby stirring
15. customfor 1 h
16. filtrationAfter air pump filtration the cake
17. washwas rinsed by water
18. additionby the mixture of water and ethanol (1:1)
19. customdried by air pump
20. dry with materialWith phosphorus pentoxide as an auxiliary desiccant, the cake was dried by vacuum (−0.095 MPa) at about 50° C.