反应详情

温度

100 °C

69.7 g of 2-chloro-5-methyl-1-trityl-1,5-dihydroimidazo[4,5-d]pyridazin-4-one was combined with 153.4 g of t-butyl piperazine-1-carboxylate, and the mixture was stirred and heated to 100° C. under nitrogen atmosphere. When the reaction mixture became easily stirrable, the temperature was raised to 150° C. The mixture was kept at this temperature for one hour. The reaction solution allowed to cool and then suspended in 250 ml of t-butyl methyl ether. The suspended material was collected by filtration. The solid was washed twice with 200 ml of t-butyl methyl ether and three times with 200 ml of water. The solid was again washed twice with 200 ml of t-butyl methyl ether, and dried to give 50.3 g of the title compound.

1. temperaturethe temperature was raised to 150° C
2. temperatureto cool
3. filtrationThe suspended material was collected by filtration
4. washThe solid was washed twice with 200 ml of t-butyl methyl ether and three times with 200 ml of water
5. washThe solid was again washed twice with 200 ml of t-butyl methyl ether
6. customdried