反应详情

温度

50 °C

44 g (0.21 moles) of 4-tert-butyl-benzenesulfonamide, 72 g (0.21 moles) of 4,6-dichloro-5-(2-methoxy-phenoxy)-[2,2′]bipyrimidine and 0.7 g of tetrabutylammonium bromide are added to a suspension of 35 g (0.25 moles) of potassium carbonate in 720 ml of methyl isobutyl ketone (MIBK), kept in an inert atmosphere (nitrogen). Once the addition is complete, the suspension is heated to reflux, operating so as to azeotropically remove the water that forms during the reaction. The reaction is kept at reflux for 5 hours. Once the reaction is complete, the suspension is cooled to 50° C. and diluted with 0.2 liters of water. Hydrochloric acid 35% is then added until obtaining a pH between 2.0 and 3.0. The suspension is cooled to 5° C./10° C. and the product is left to crystallise for 10 hours. The suspension is filtered and 120 g in wet form of the title compound are obtained equal to 100 g in dry form (0.19 moles) (yield 92%; purity 99.6% HPLC).

1. additionOnce the addition
2. temperaturethe suspension is heated
3. temperatureto reflux
4. customto azeotropically remove the water that
5. customforms during the reaction
6. temperatureat reflux for 5 hours
7. customuntil obtaining a pH between 2.0 and 3.0
8. temperatureThe suspension is cooled to 5° C./10° C.
9. waitthe product is left
10. customto crystallise for 10 hours
11. filtrationThe suspension is filtered