反应详情

温度

110 °C

0.70 g of toluene-4-sulfonic acid 1-(3-chloro-4-fluorobenzoyl)-4-fluoropiperidin-4-yl-methyl ester (1.57 mmol), 0.308 g of sodium azide (4.70 mmol) and 0.20 g of tetrabutylammonium azide (0.70 mmol) are mixed in 3.50 ml of dimethyl sulfoxide. The mixture is heated at 110° C. under a nitrogen atmosphere for 20 hours. The reaction mixture is poured into ice-cold water and then extracted with ethyl acetate. The organic phase is washed with water and then with a saturated aqueous solution of sodium chloride, dried over magnesium sulfate, filtered and concentrated under vacuum. The title product is isolated by chromatography on a neutral alumina column (eluent: hexane/ethyl acetate; 70:30). 0.313 g of a yellow oil is obtained.

1. additionThe reaction mixture is poured into ice-cold water
2. extractionextracted with ethyl acetate
3. washThe organic phase is washed with water
4. dry with materialwith a saturated aqueous solution of sodium chloride, dried over magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated under vacuum