反应详情

3-Amino-1,2,4-triazole (4.2 g, 0.05 mol) and ethyl-2-chloro-acetoacetate (12.64 g, 0.0768 mol) were refluxed in acetic acid (15 ml) under a nitrogen atmosphere. The reaction mixture first turned into a clear yellow solution and after about 15 minutes a solid started precipitating. Reflux continued for one hour. The crude product was filtered off, washed with hot methanol (2×10 ml), and dried in an oven at 90° C. to give 5.9 g (64%) of pure TAI-3. TLC (in Et2O/MeOH, 70:30 v/v) showed only one spot. The compound is soluble in hot DMF and DMSO. mp=starts darkening at ˜308° C. and decomposes at temperatures >325° C.

1. customa solid started precipitating
2. temperatureReflux
3. waitcontinued for one hour
4. filtrationThe crude product was filtered off
5. washwashed with hot methanol (2×10 ml)
6. customdried in an oven at 90° C.
7. customto give 5.9 g (64%) of pure TAI-3
8. customstarts darkening at ˜308° C.
9. customdecomposes at temperatures >325° C.