反应详情

To a solution of 1.38 g of 3-(N,N-dimethylamino-methylene)aminosulfonyl-2,2-diethyl-1-propanol in 30 ml of tetrahydrofuran was added 0.23 g of 60% sodium hydride in oil and the mixture was stirred at room temperature for 1 hour. To this reaction mixture was added 0.74 g of 6-chloro-7-methyl[1,2,4]triazolo[1,5-b]pyridazine and the mixture was refluxed with stirring for 1 hour. After cooling, the reaction mixture was adjusted to pH 6 with 1N-hydrochloric acid and extracted with ethyl acetate-tetrahydrofuran (1:1). The extract was washed with water and dried and the solvent was distilled off. To the residue was added 14 ml of 6N-hydrochloric acid and the mixture was stirred at 110° C. for 30 minutes. After cooling, 100 ml of water was added to the reaction mixture and the resulting crystals were recovered by filtration and recrystallized from methanol to provide 1.16 g of the title compound. m.p. 208°-209° C.

1. temperaturethe mixture was refluxed
2. stirringwith stirring for 1 hour
3. temperatureAfter cooling
4. extractionextracted with ethyl acetate-tetrahydrofuran (1:1)
5. washThe extract was washed with water
6. customdried
7. distillationthe solvent was distilled off
8. additionTo the residue was added 14 ml of 6N-hydrochloric acid
9. stirringthe mixture was stirred at 110° C. for 30 minutes
10. temperatureAfter cooling
11. addition100 ml of water was added to the reaction mixture
12. filtrationthe resulting crystals were recovered by filtration
13. customrecrystallized from methanol