反应详情

温度

17.5 °C

Potassium tert-butoxide (10.3 g, 92.5 mmol) in tetrahydrofuran (25 mL) was stirred at 23 to 27° C. for 30 minutes, and dimethyl carbonate (4.67 mL, 55.5 mmol) was added while the temperature was kept at 35° C. or below. To the reaction mixture, 3-amino-4-methylpyridine (5.00 g, 46.2 mmol) in tetrahydrofuran (40 mL) stirred at 32 to 38° C. for 90 minutes was added dropwise at 20 to 35° C. over 2 hours with stirring. The resulting reaction mixture was cooled to 15 to 20° C., stirred with water (25 mL) at 25° C. or below for 1 hour and extracted with tetrahydrofuran. The organic layer was azeotropically distilled with toluene under reduced pressure to a volume of about 50 mL and stirred at 23 to 27° C. for one day. The precipitated solid was collected by filtration, washed with toluene and dried under reduced pressure to give the title compound as a brown solid (6.77 g, yield 88%).

1. customwas kept at 35° C. or below
2. additionwas added dropwise at 20 to 35° C. over 2 hours
3. customThe resulting reaction mixture
4. extractionextracted with tetrahydrofuran
5. distillationThe organic layer was azeotropically distilled with toluene under reduced pressure to a volume of about 50 mL
6. stirringstirred at 23 to 27° C. for one day
7. filtrationThe precipitated solid was collected by filtration
8. washwashed with toluene
9. customdried under reduced pressure