反应详情

温度

60 °C

To a suspension of 2.8 g of 3,6-dimethylimidazo [2,1-b]thiazole-5-sulfonic acid in 3.4 ml of phophorus oxychloride, 1.8 g of tri-n-propylamine is added under cooling and stirred for 30 minutes at 60° C. The reaction solution after cooling is poured into ice water and extracted with dichloromethane. The dichloromethane layer is collected, dried and then distilled to remove dichloromethane. The residue is dissolved in 35 ml of acetonitrile, to which 3.8 ml of aqueous ammonia is added under cooling and stirred for 30 minutes at room temperature. The acetonitrile is distilled off under reduced pressure, and to the residue is added water. The precipitated crystalline solid is collected by filtration and washed with tetrachloromethane to give 1.5 g of the title compound as colorless crystals. mp. 177°-178° C.

1. additionis added
2. temperatureunder cooling
3. temperatureThe reaction solution after cooling
4. extractionextracted with dichloromethane
5. customThe dichloromethane layer is collected
6. customdried
7. distillationdistilled
8. customto remove dichloromethane
9. dissolutionThe residue is dissolved in 35 ml of acetonitrile, to which 3.8 ml of aqueous ammonia
10. additionis added
11. temperatureunder cooling
12. stirringstirred for 30 minutes at room temperature
13. distillationThe acetonitrile is distilled off under reduced pressure
14. additionto the residue is added water
15. filtrationThe precipitated crystalline solid is collected by filtration
16. washwashed with tetrachloromethane