Synthesis of 3,3＇,4,4＇-tetrahydro-4,4＇-bibenzo[e][1,3]oxazine-2,2＇-diones via reaction of salicylidendphenylhy- drazone and triphosgene with the aid of low-valent titanium reagent is described. This method has the...Synthesis of 3,3＇,4,4＇-tetrahydro-4,4＇-bibenzo[e][1,3]oxazine-2,2＇-diones via reaction of salicylidendphenylhy- drazone and triphosgene with the aid of low-valent titanium reagent is described. This method has the advantages of accessible starting materials, good yields and short reaction time.展开更多
The title compound （C28H19Cl2N） has been synthesized by the reaction of dibenzoylmethane and N-（4-chlorobenzylidene）-4-chlorobenzenamine promoted by low-valent titanium reagent, and characterized by elemental anal...The title compound （C28H19Cl2N） has been synthesized by the reaction of dibenzoylmethane and N-（4-chlorobenzylidene）-4-chlorobenzenamine promoted by low-valent titanium reagent, and characterized by elemental analysis, IR, ^1H NMR and X-ray single-crystal diffraction. The crystal belongs to monoclinic, space group P2 1/C with a = 9.952（2）, b = 9.863（2）, c = 23.460（6） A, β = 99.62（2）°, V = 2270.4（9） A^3, Mr = 440.34, Z = 4, Dc = 1.288 g/cm^3, μ（MoKa） = 0.301 mm^-1, F（000） = 912, the final R = 0.0387 and wR = 0.0793. X-ray analysis reveals that the four phenyl rings in the pyrrole ring are not coplanar.展开更多
基金Project supported by the National Natural Science Foundation of China （No. 21072144） and the Major Basic Research Project of the Natural Science Foundation of the Jiangsu Higher Education Institutions （No. 10KJAI50049）.
文摘Synthesis of 3,3＇,4,4＇-tetrahydro-4,4＇-bibenzo[e][1,3]oxazine-2,2＇-diones via reaction of salicylidendphenylhy- drazone and triphosgene with the aid of low-valent titanium reagent is described. This method has the advantages of accessible starting materials, good yields and short reaction time.
基金This work was supported by the Natural Science Foundation of Jiangsu Education Department (No. 03KJB 150136)
文摘The title compound （C28H19Cl2N） has been synthesized by the reaction of dibenzoylmethane and N-（4-chlorobenzylidene）-4-chlorobenzenamine promoted by low-valent titanium reagent, and characterized by elemental analysis, IR, ^1H NMR and X-ray single-crystal diffraction. The crystal belongs to monoclinic, space group P2 1/C with a = 9.952（2）, b = 9.863（2）, c = 23.460（6） A, β = 99.62（2）°, V = 2270.4（9） A^3, Mr = 440.34, Z = 4, Dc = 1.288 g/cm^3, μ（MoKa） = 0.301 mm^-1, F（000） = 912, the final R = 0.0387 and wR = 0.0793. X-ray analysis reveals that the four phenyl rings in the pyrrole ring are not coplanar.
