反应详情

温度

120 °C

In a pressure tube 2-(benzyloxy)-5-nitroaniline (0.65 g), 2,4-dichloro-5-fluoropyrimidine (0.66 g) and DIPEA (0.69 g) were taken in n-butanol (10 mL). The reaction mixture was heated at 120° C. for 24 hr. The reaction was monitored on TLC using DCM:hexane:ethyl acetate (3:5:2) as mobile phase. The reaction was complete after 24 h. After completion, reaction mixture was allowed to cool at room temperature. The reaction was poured into water and extracted with ethyl acetate (3×25 mL). The ethyl acetate layer washed with brine solution, dried over sodium sulfate and concentrated under reduced pressure at 40° C. Crude material was purified by triturating with diethyl ether to give 0.25 g of N-(2-(benzyloxy)-5-nitrophenyl)-2-chloro-5-fluoropyrimidin-4-amine. M+1=374.8.

1. customAfter completion, reaction mixture
2. temperatureto cool at room temperature
3. extractionextracted with ethyl acetate (3×25 mL)
4. washThe ethyl acetate layer washed with brine solution
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated under reduced pressure at 40° C
7. customCrude material was purified
8. customby triturating with diethyl ether