反应详情

2-Chloro-isonicotinonitrile (80 g, 0.58 mol) and piperazine (199 g, 2.32 mol, 5 equiv) were combined and heated at 70 DC for 2.5 hours. The resulting suspension was cooled to room temperature and partitioned between a solution of 50% ethyl acetate/dichloromethane and water. The organic phase was separated, and the aqueous phase was extracted with dichloromethane. The combined organic phases were concentrated in vacuo to about half the initial volume and ether was added. The suspension was stirred overnight, then filtered. The solid was dried under vacuum to give the desired product (31 g). The mother liquors were concentrated in vacuo and the residue was triturated with ether and filtered. The solid collected in this second batch was dried under vacuum and combined with the first batch to give the total amount of desired product (46 g, 42%).

1. temperatureheated at 70 DC for 2.5 hours
2. custompartitioned between a solution of 50% ethyl acetate/dichloromethane and water
3. customThe organic phase was separated
4. extractionthe aqueous phase was extracted with dichloromethane
5. concentrationThe combined organic phases were concentrated in vacuo to about half the initial volume and ether
6. additionwas added
7. filtrationfiltered
8. customThe solid was dried under vacuum