摘要
The reaction of hydrazine hydrate with a new α,γ-diketone ester 3, derived from the reaction of 2,6-dimethyl-3,5-diacetyl-pyridine 2 with diethyl oxalate in the presence of sodium ethoxide, afforded the pyrazole derivative 4. Treatment of 4 with 2-chlorobenzoyl chloride gave diethyl 2,6-dimethyl-3,5-diyl-(1-2(chlorobenzoyl)-1H-pyrazole-3-diethyl-carboxylate) pyridine 5. Fine crystal of 5 suitable for XRD analysis was obtained form recrystalization in ethyl acetate. The crystal belongs to the triclinic system, space group P1^-, with a = 1.0342(11), b = 1.2211(12), c = 1.5013(15) nm, α = 82.5190(10),β = 85.7960(10),γ = 85.3150(10)°, V= 1.8697(3) nm^3, Dc= 1.173 g/cm^3, μ = 0.219 mm^-1, F(000) = 684, Z = 2, the final R = 0.0720 and wR = 0.2211.
The reaction of hydrazine hydrate with a new α,γ-diketone ester 3, derived from the reaction of 2,6-dimethyl-3,5-diacetyl-pyridine 2 with diethyl oxalate in the presence of sodium ethoxide, afforded the pyrazole derivative 4. Treatment of 4 with 2-chlorobenzoyl chloride gave diethyl 2,6-dimethyl-3,5-diyl-(1-2(chlorobenzoyl)-1H-pyrazole-3-diethyl-carboxylate) pyridine 5. Fine crystal of 5 suitable for XRD analysis was obtained form recrystalization in ethyl acetate. The crystal belongs to the triclinic system, space group P1^-, with a = 1.0342(11), b = 1.2211(12), c = 1.5013(15) nm, α = 82.5190(10),β = 85.7960(10),γ = 85.3150(10)°, V= 1.8697(3) nm^3, Dc= 1.173 g/cm^3, μ = 0.219 mm^-1, F(000) = 684, Z = 2, the final R = 0.0720 and wR = 0.2211.
基金
the Key Subject of Shanghai Municipal Education Commission(J50102)
the Foundation of Education Commission of Shanghai Municipality(08zz44)