反应详情

13.87 g (100.35 mmol) of potassium carbonate are added to 21.50 g (91.2 mmol) of 5-(4-chlorophenyl)-4-allyl-2,4-dihydro-3H-1,2,4-triazol-3-one from Example 210A and 11.88 g (109.5 mmol) of methyl chloroacetate in 350 ml acetonitrile and the mixture is heated under reflux for 5 hrs with stirring. It is then concentrated and the residue taken up in ethyl acetate is washed with 1 N hydrochloric acid and then with saturated sodium chloride solution. The organic phase is dried over sodium sulphate. After filtration, the filtrate is concentrated in vacuo. After purification by flash chromatography on silica gel (eluent: cyclohexane/ethyl acetate 2:1) 24.00 g (85% of theory) of the target compound are obtained.

1. temperaturethe mixture is heated
2. temperatureunder reflux for 5 hrs
3. concentrationIt is then concentrated
4. washis washed with 1 N hydrochloric acid
5. dry with materialThe organic phase is dried over sodium sulphate
6. filtrationAfter filtration
7. concentrationthe filtrate is concentrated in vacuo
8. customAfter purification by flash chromatography on silica gel (eluent: cyclohexane/ethyl acetate 2:1) 24.00 g (85% of theory) of the target compound
9. customare obtained