反应详情

温度

170 °C

A mixture of N-[1-pyrimidin-5-yl-meth-(E)-ylidene]-N′-(3-trifluoromethoxy-phenyl)-hydrazine (215 mg, 0.76 mmol) and zinc chloride (208 mg, 1.52 mmol) in 2 ml ethyl acetoacetate was heated at 170° C. for 3 h and stirring was continued for 20 h at room temperature. Ethyl acetoacetate was distilled (Kugelrohr distillation, 90° C., 10-40 mbar) and the residue was purified by column chromatography (EtOAc:n-heptane 4:1) to afford the title compound as a yellow oil (89 mg, 30%). MS: 393.0 (MH+).

1. distillationEthyl acetoacetate was distilled
2. distillation(Kugelrohr distillation, 90° C., 10-40 mbar)
3. customthe residue was purified by column chromatography (EtOAc:n-heptane 4:1)