反应详情

温度

0 °C

A solution of 3.6 ml (49.8 mmol) of thionyl chloride in 30 ml of dichloromethane is added dropwise at room temperature to a solution of 15.0 g (38.3 mmol) of {3-methyl-4-[3-(3-nitroimidazo[1,2-b]pyridazin-6-yl-sulfanyl)propylsulfanyl]pyridin-2-yl}methanol in 400 ml of anhydrous dichloromethane and the mixture is then stirred for a further 18 h. It is then cooled to 0° C. and aqueous sodium carbonate solution (100 ml) is cautiously added dropwise. The dichloromethane is distilled off. The suspension is then treated with 400 ml of water and stirred at 0° C. for 30 min. The precipitate is filtered off, washed with water, dried at 40° C. in vacuo and then suspended in 300 ml of acetone. After filtration and drying, 15.3 g (97%) of the title compound are isolated as a beige powder. M.p.: 155-156° C.

1. distillationThe dichloromethane is distilled off
2. additionThe suspension is then treated with 400 ml of water
3. stirringstirred at 0° C. for 30 min
4. filtrationThe precipitate is filtered off
5. washwashed with water
6. customdried at 40° C. in vacuo
7. filtrationAfter filtration
8. customdrying