反应详情

温度

115 °C

841 mg of 2-cyano-3,5-difluoropyridine, 880 mg of 2-(2-aminoethyl)pyridine and 1.658 g of potassium carbonate in 12.5 ml of dimethyl sulphoxide are introduced into a 20 ml microwave tube reactor. The mixture is then heated in a microwave for 1 and a half hours at 115° C. The reaction medium is run into 100 ml of water and 100 ml of ethyl acetate. The aqueous phase is re-extracted twice with 50 ml of ethyl acetate. The combined organic phases are washed with water and then with a saturated aqueous solution of sodium chloride, dried over sodium sulphate and concentrated under reduced pressure. After purification by flash chromatography on 70 g of silica gel, elution being carried out with a mixture of ethyl acetate and cyclohexane (40/60 by volume), and the first eluted product being recovered, 549 mg of 2-cyano-5-fluoro-3-(2-pyridin-2-ylethylamino)pyridine are thus obtained in the form of a beige powder, the characteristics of which are the following:

1. extractionThe aqueous phase is re-extracted twice with 50 ml of ethyl acetate
2. washThe combined organic phases are washed with water
3. dry with materialwith a saturated aqueous solution of sodium chloride, dried over sodium sulphate
4. concentrationconcentrated under reduced pressure
5. customAfter purification by flash chromatography
6. washon 70 g of silica gel, elution
7. additionbeing carried out with a mixture of ethyl acetate and cyclohexane (40/60 by volume)
8. customthe first eluted product being recovered