反应详情

温度

-30 °C

In a 50 mL 3-neck RBF equipped with a magnetic stirrer, calcium chloride guard tube and thermo pocket was charged N4-(3-aminophenyl)-5-fluoro-N2-(4-(2-methoxyethoxy)phenyl)pyrimidine-2,4-diamine (0.40 g) in dry DCM (10 mL) and was cooled to −30° C. An acryloyl chloride solution in DCM (0.107 g in 5.0 mL DCM) was added slowly and the reaction mixture was stirred at −30° C. for approx. 40 minutes. The reaction was monitored on TLC using chloroform:methanol (9.6:0.4) as mobile phase. The reaction mixture was poured into water (100 mL) and basified using sodium bicarbonate. The reaction mixture was extracted with MDC (2×25 mL) and the combined organic layer was washed with 50 mL brine solution. The organic layer was dried over sodium sulfate and concentrated completely under reduce pressure at 40° C. Obtained solid was purified by triturating with diethyl ether (2×mL) and dried under vacuum to give 0.28 g N-(3-((5-fluoro-2-((4-(2-methoxyethoxy)phenyl)amino)pyrimidin-4-yl)amino)phenyl)acrylamide.

1. customIn a 50 mL 3-neck RBF equipped with a magnetic stirrer, calcium chloride guard tube
2. extractionThe reaction mixture was extracted with MDC (2×25 mL)
3. washthe combined organic layer was washed with 50 mL brine solution
4. dry with materialThe organic layer was dried over sodium sulfate
5. concentrationconcentrated completely
6. customat 40° C
7. customObtained solid
8. customwas purified
9. customby triturating with diethyl ether (2×mL)
10. customdried under vacuum