反应详情

温度

60 °C

To a solution of 7-(4-chlorophenyl)-5-methyl-2-((6-(trifluoromethyl)pyridin-3-yl)methyl)-[1,2,4]triazolo[4,3-c]pyrimidin-3(2H)-one (210 mg, 0.50 mmol) in dichloromethane (10 mL) and methanol (10 mL) at room temperature under argon was added calcium carbonate (50.0 mg, 0.50 mmol) and N,N,N-trimethyl-1-phenylmethanaminium tribromide (195 mg, 0.50 mmol). The resulting suspension was stirred and heated at 60° C. under argon for 1 h. Analysis by HPLC/MS indicated that the starting material had been consumed. The solvents were removed under reduced pressure, and water (25 mL) was added. After stirring at room temperature for 30 min, the solid product was collected by filtration and further washed with water (2×10 mL). After drying, the title compound (273 mg) was obtained as an off-white solid. HPLC/MS: retention time=3.84 min, [M+H]30 =500.

1. customhad been consumed
2. customThe solvents were removed under reduced pressure, and water (25 mL)
3. additionwas added
4. stirringAfter stirring at room temperature for 30 min
5. filtrationthe solid product was collected by filtration
6. washfurther washed with water (2×10 mL)
7. customAfter drying