反应详情

4.1 g (31.9 mmol) of ethyl azidoacetate and 2.8 g (31.9 mmol) of 2-chloroacrylonitrile are stirred in 32 ml of water at a bath temperature of 80° C. for 16 h. After cooling to RT, the solution is acidified with 1 N hydrochloric acid and extracted with ethyl acetate. The organic phase is dried over sodium sulphate, filtered and concentrated under reduced pressure. 50 ml of ethanol and 10 drops of concentrated sulphuric acid are added to the residue, and the mixture is stirred under reflux for 16 h. For work-up, the reaction mixture is concentrated under reduced pressure, ethyl acetate is added to the residue, the suspension is washed with semiconcentrated sodium bicarbonate solution and the organic phase is dried over sodium sulphate. The solvent is removed completely on a rotary evaporator and the solid is dried under reduced pressure. Yield: 1.5 g (25% of theory)

1. extractionextracted with ethyl acetate
2. dry with materialThe organic phase is dried over sodium sulphate
3. filtrationfiltered
4. concentrationconcentrated under reduced pressure
5. addition50 ml of ethanol and 10 drops of concentrated sulphuric acid are added to the residue
6. temperatureunder reflux for 16 h
7. concentrationFor work-up, the reaction mixture is concentrated under reduced pressure, ethyl acetate
8. additionis added to the residue
9. washthe suspension is washed with semiconcentrated sodium bicarbonate solution
10. dry with materialthe organic phase is dried over sodium sulphate
11. customThe solvent is removed completely on a rotary evaporator
12. customthe solid is dried under reduced pressure