反应详情

To a solution of 6.18 g of 5-bromo-6-methyl-1H-indazole and 15 g of tert-butyl-3-[(tosyl-oxy)methyl]azetidin-1-carboxylate in 200 ml DMF were added 9.54 g of caesium carbonate and 10.8 g of tetrabutylammonium iodide at 25° C., and this was then heated under reflux for 1.5 hrs. After cooling, the reaction mixture was treated with 1:1 hexane/ether and water, the phases separated and the aqueous phase extracted twice with 250 ml portions of 1:1 hexane/ether. The combined organic phases were washed with saturated sodium chloride solution, dried over sodium sulphate, and concentrated in vacuo after filtration.

1. temperaturethis was then heated
2. temperatureunder reflux for 1.5 hrs
3. temperatureAfter cooling
4. customthe phases separated
5. extractionthe aqueous phase extracted twice with 250 ml portions of 1:1 hexane/ether
6. washThe combined organic phases were washed with saturated sodium chloride solution
7. dry with materialdried over sodium sulphate
8. concentrationconcentrated in vacuo
9. filtrationafter filtration