反应详情

温度

117 °C

A 5 L, 4-neck, round-bottomed flask fitted with a mechanical stirrer, digital thermometer, heating and cooling capabilities, condenser, addition funnel, and nitrogen inlet and outlet, was flushed with nitrogen and charged with 479.8 g (2.15 moles) of 2-chloro-N-cyclobutyl-9H-purin-6-amine, 387.5 g (2.36 moles) of N-(4-aminophenyl)-N-methyl-acetamide, and 3.6 L of dry 1-butanol. The mixture was stirred and 2.72 mL (0.02 moles) of chlorotrimethylsilane was added at 25° C. The mixture was heated to 117° C. over about 50 minutes. The reaction temperature and stirring was maintained for 12.5 hours. The mixture was cooled to 50° C. over a period of 2 hours. A temperature of 50° C. was maintained for an additional hour. The product was filtered and the filter cake was washed three times with a total of 1.2 L of 1-butanol. The filter cake was collected and dried at 50° C./20 mm Hg for 24 hours to give 514.3 g of light yellow crystalline solid. Theoretical yield was 832.0 g. Actual yield was 61.8%.

1. customA 5 L, 4-neck, round-bottomed flask fitted with a mechanical stirrer
2. temperaturedigital thermometer, heating
3. temperaturecooling
4. additioncapabilities, condenser, addition funnel, and nitrogen inlet and outlet
5. customwas flushed with nitrogen
6. stirringThe reaction temperature and stirring
7. temperaturewas maintained for 12.5 hours
8. temperatureThe mixture was cooled to 50° C. over a period of 2 hours
9. temperatureA temperature of 50° C. was maintained for an additional hour
10. filtrationThe product was filtered
11. washthe filter cake was washed three times with a total of 1.2 L of 1-butanol
12. customThe filter cake was collected
13. customdried at 50° C./20 mm Hg for 24 hours