反应详情

温度

75 °C

A 12 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 492.9 g (2.61 moles) of 2,6-dichloro-9H-purine, 497.7 mL (2.87 moles) of N,N-diisopropylethylamine, and 3.65 L of anhydrous 1-butanol. The mixture was stirred and heated to 75° C. and 244.9 mL (2.87 moles) of cyclobutylamine in 1.25 L of anhydrous 1-butanol, was added during about 1 hour at a temperature of 75° C.-77° C. The reaction temperature and stirring was maintained for 4.5 hours. The mixture was cooled to 5° C. over a period of 1 hour. The product was filtered and the filter cake was washed three times with a total of 0.9 L of 1-butanol. The filter cake was collected and dried at 75° C./20 mm Hg for 24 hours to give 506.6 g of light yellow crystalline solid. Theoretical yield was 583.3 g. Actual yield was 86.9%.

1. customA 12 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 4.5 hours
8. temperatureThe mixture was cooled to 5° C. over a period of 1 hour
9. filtrationThe product was filtered
10. washthe filter cake was washed three times with a total of 0.9 L of 1-butanol
11. customThe filter cake was collected
12. customdried at 75° C./20 mm Hg for 24 hours