反应详情

5.2 g (40.0 mmol) 6-chloropyridin-3-ol, 11.9 g (60.0 mmol) 1-iodo-2,2-dimethylpropane, 19.6 g (60.0 mmol) cesium carbonate and 120 ml diethylene glycol dimethyl ether are divided into five portions of equal size and are reacted in portions at 160° C. for 4 h in a single mode microwave (CEM Explorer). Thereafter, the five reaction mixtures obtained are combined, the solid is filtered off and rinsed with diethylene glycol dimethyl ether and the filtrate and wash solutions are combined. The majority of the solvent is removed and 300 ml water are added to the concentrated solution (approx. 50 ml). The mixture is stirred for 30 min and the solid obtained is filtered off, washed once with water and dried under a high vacuum.

1. customare reacted in portions at 160° C. for 4 h in a single mode microwave (CEM Explorer)
2. customThereafter, the five reaction mixtures
3. customobtained
4. filtrationthe solid is filtered off
5. washrinsed with diethylene glycol dimethyl ether
6. washthe filtrate and wash solutions
7. customThe majority of the solvent is removed
8. addition300 ml water are added to the concentrated solution (approx. 50 ml)
9. customthe solid obtained
10. filtrationis filtered off
11. washwashed once with water
12. customdried under a high vacuum