反应详情

4-BROMO-3-CHLOROBENZENESULFONYL CHLORIDE (10.0 g, 0.0345 mol) and 2-AMINOTHIAZOLE (3.80 g, 0.0379 mol) were mixed in Pyridine (40 mL, 0.5 mol). The reaction was allowed to stir at room temperature for 9 days. The reaction was concentrated in vacuo to a total volume of approximately 40 mL. The residue was triturated with acetonitrile and the solid collected by filtration. The filtrate was concentrated in vacuo and the residue triturated with 1N HCl. The solid was collected by filtration and rinsed with acetonitrile then ethyl ether. The combined solid from steps 4 and 5 was dissolved in boiling acetonitrile and treated with activated carbon then filtered through a celite pad. The filtrate was reduced to ⅓ its original volume by distillation. The mixture was cooled to room temperature. The crystals were collected by filtration and rinsed with ethyl ether. Vacuum drying gave 7.73 g of yellow solid.

1. concentrationThe reaction was concentrated in vacuo to a total volume of approximately 40 mL
2. customThe residue was triturated with acetonitrile
3. filtrationthe solid collected by filtration
4. concentrationThe filtrate was concentrated in vacuo
5. customthe residue triturated with 1N HCl
6. filtrationThe solid was collected by filtration
7. washrinsed with acetonitrile
8. dissolutionThe combined solid from steps 4 and 5 was dissolved
9. additiontreated with activated carbon
10. filtrationthen filtered through a celite pad
11. distillationby distillation
12. temperatureThe mixture was cooled to room temperature
13. filtrationThe crystals were collected by filtration
14. washrinsed with ethyl ether
15. customVacuum drying