反应详情

温度

100 °C

A mixture of N4-[(trans-4-aminocyclohexyl)methyl]-5-nitro-N2-[2-(trifluoromethoxy)benzyl]pyrimidine-2,4-diamine (124 mg, 0.28 mmol), (S)-3-oxiranyl-pyridine (34 mg, 0.28 mmol) and lithium perchlorate (60 mg, 0.56 mmol) in CH3CN was heated to 100° C. in a sealed tube and stirred for 1 h. The reaction mixture was concentrated and diluted with ethyl acetate. The solution was then treated with 1M Na2CO3 and the organic phase was separated. The aqueous phase was re-extracted with ethyl acetate (×2). The combined organic phase was dried over Na2SO4 and concentrated. The resulting residue was purified by silica gel prep TLC using 10:1:0.05 CH2Cl2:MeOH:NH4OH as an eluent to afford 15 mg of the title compound as an off-white solid (10%), m/z 562.7 [M+1]+.

1. concentrationThe reaction mixture was concentrated
2. additiondiluted with ethyl acetate
3. additionThe solution was then treated with 1M Na2CO3
4. customthe organic phase was separated
5. extractionThe aqueous phase was re-extracted with ethyl acetate (×2)
6. dry with materialThe combined organic phase was dried over Na2SO4
7. concentrationconcentrated
8. customThe resulting residue was purified by silica gel prep TLC