反应详情

温度

0 °C

To a stirred solution of 3-chloro-N-isopropyl-5-methoxy-N-(2-methylcarbamoyl-ethyl)-benzamide (0.312 g) in anhydrous dichloromethane (5.0 ml) was added sodium azide (0.065 g) and the mixture cooled to 0° C. Trifluoromethanesulphonic anhydride (0.200 ml) was added and the reaction stirred at room temperature for 18 h. The reaction mixture was partitioned between ethyl acetate and water. The aqueous layer was removed and the organic layer dried with brine and over sodium sulphate and concentrated under reduced pressure. The residue was purified by flash column chromatography, eluting with ethyl acetate:petroleum ether (4:1 v/v); to give the title compound as a white solid (0.121 g).

1. customThe reaction mixture was partitioned between ethyl acetate and water
2. customThe aqueous layer was removed
3. dry with materialthe organic layer dried with brine and over sodium sulphate
4. concentrationconcentrated under reduced pressure
5. customThe residue was purified by flash column chromatography
6. washeluting with ethyl acetate:petroleum ether (4:1 v/v)