反应详情

温度

70 °C

To a solution of 1.57 g of 3-chloro-1-propanesulfonamide in 20 ml of methanol was added 20 ml of 2N-potassium hydrogensulfide, followed by heating at 70° C. for 50 minutes. Further, 1.48 g of 28% sodium methoxide-methanol solution and 1.32 g of 2,6-dichloroimidazo[1,2-b]pyridazine [Japanese Unexamined Patent Publication No. SHO 64(1989)-38092] were added to the reaction mixture, and refluxed at 100° C. for 3 hours. The mixture was concentrated under reduced pressure. Then, the residue to which was 20 ml of water was added was adjusted to pH 7.0 with 1N-hydrochloric acid. The precipitated crystals were collected by filtration and subjected to a silica gel column chromatography, eluting with chloroform and methanol (50:1). The corresponding combined fractions were concentrated, and the residue was recrystallized to obtain 1.1 g of the title compound.

1. temperaturerefluxed at 100° C. for 3 hours
2. concentrationThe mixture was concentrated under reduced pressure
3. additionwas added
4. filtrationThe precipitated crystals were collected by filtration
5. washeluting with chloroform and methanol (50:1)
6. concentrationThe corresponding combined fractions were concentrated
7. customthe residue was recrystallized