反应详情

温度

120 °C

In a pressure tube tert-butyl(3-aminophenyl)(methyl)carbamate (2.0 g), 2,4-dichloro-5-fluoropyrimidine (2.25 g) and DIPEA (2.32 g) were added in 1-butanol (15 ml). The reaction mixture was heated at 120° C. for 3 hr. The reaction was monitored on TLC using hexane:ethyl acetate (7:3) as mobile phase. The reaction was complete after 3 hr. After completion of the reaction, the reaction mixture was allowed to cool at room temperature. The reaction mixture was poured into water and extracted with ethyl acetate (3×25 ml). Ethyl acetate layer washed with brine solution, dried over sodium sulfate and concentrated under reduced pressure at 40° C. Crude material was purified by using Combiflash chromatography. Product was eluted with 14.8% ethyl acetate in hexane to give 1.93 g of tert-butyl (3-((2-chloro-5-fluoropyrimidin-4-yl)amino)phenyl)(methyl)carbamate. M+1=466.8.

1. customAfter completion of the reaction
2. temperatureto cool at room temperature
3. extractionextracted with ethyl acetate (3×25 ml)
4. washEthyl 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. washProduct was eluted with 14.8% ethyl acetate in hexane