反应详情

温度

60 °C

To a solution of [9-chloro-1-(6-methoxy-2-methylpyridin-3-yl)-1,2,3,4-tetrahydropyrimido[1,2-a]benzimidazol-6-yl](cyclopropyl)methanol (111.5 mg, 0.280 mmol) in tetrahydrofuran (2.8 mL) was added 1,1′-(azodicarbonyl)dipiperidine (141.1 mg, 0.559 mmol) and tributylphosphine (139.3 μL, 0.559 mmol). After 10 min, to the mixture was added 2,2,2-trifluoroethanol (204.0 μL, 2.800 mmol). The reaction mixture was stirred at 60° C. for 2 hrs. The mixture was concentrated. To the residue was added diethyl ether and the precipitate was removed by filtration. The residue was purified by silica gel column chromatography eluting with a 0-50% ethyl acetate/n-hexane gradient mixture. The resulting solid was recrystallized from ethyl acetate/n-hexane to give the title compound as a colorless powder (92.4 mg, 0.192 mmol, 69%).

1. concentrationThe mixture was concentrated
2. additionTo the residue was added diethyl ether
3. customthe precipitate was removed by filtration
4. customThe residue was purified by silica gel column chromatography
5. washeluting with a 0-50% ethyl acetate/n-hexane gradient mixture
6. customThe resulting solid was recrystallized from ethyl acetate/n-hexane