Ethyl 2-chloroacetoacetate → HCID 178418931、化合物

関与物質

反応手順

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.

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