反应详情

To 40 ml of thionyl chloride were added 2.93 g of 1-chloro-5-isoquinolinesulfonic acid as obtained in Example 1 and 0.4 ml of N,N-dimethylformamide. Then, the resulting mixture was refluxed while heating at 80° to 85° C. for 2 hours, followed by removal of the thionyl chloride under reduced pressure. Subsequently, 10 ml of dichloromethane was added to the reaction mixture to precipitate crystals, followed by separation of the crystals by filtration. The crystals thus obtained were washed with 10 ml of dichloromethane, and then dried under reduced pressure to obtain 3.06 g of 1-chloro-5-isoquinolinesulfonyl chloride hydrochloride. The compound was analyzed to give the following data.

1. temperatureThen, the resulting mixture was refluxed
2. temperaturewhile heating at 80° to 85° C. for 2 hours
3. customfollowed by removal of the thionyl chloride under reduced pressure
4. additionSubsequently, 10 ml of dichloromethane was added to the reaction mixture
5. customto precipitate crystals
6. customfollowed by separation of the crystals by filtration
7. customThe crystals thus obtained
8. washwere washed with 10 ml of dichloromethane
9. customdried under reduced pressure