The title compound, 2-（3-silatranylpropylamino）-4-dichlorophenyl-5,5-dimethyl- 1,3,2-dioxaphosphorinane-2-oxide （2（C20H33N2O6Psi）？C2H6O？CH4O, Mr = 991.20）, has been synthe- sized by the nucleophilic substituti...The title compound, 2-（3-silatranylpropylamino）-4-dichlorophenyl-5,5-dimethyl- 1,3,2-dioxaphosphorinane-2-oxide （2（C20H33N2O6Psi）？C2H6O？CH4O, Mr = 991.20）, has been synthe- sized by the nucleophilic substitution reaction of 2-chloro-4-phenyl-5,5-dimethyl-1,3,2-dioxa- phosphorinane-2-oxide with γ-aminopropylsilatrane, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P with a = 10.3783（15）, b = 11.2402（17）, c = 12.1675（18） ？, ？ = 70.653（4）, ？ = 82.908（4）, ？ = 85.690（4）？, V = 1328.1（3） ？3, Z = 1, Dc = 1.239 g/cm3, μ = 0.19 mm？1, F（000） = 532, the final R = 0.0640 and wR = 0.2090 for 3615 observed reflections with I 〉 2？（I）. The cyclic dioxaphosphorinane ring in the molecule adopts a thermodynamically stable cis conformation, while the silatrane fragment forms a cage-like structure in which there exists an intramolecular Si？N donor-acceptor bond. In the crystal structure, centrosymmetrically related molecules are linked by pairs of N–H？？？O hydrogen bonds into dimers, generating rings with graph-set motif R22（8）. Furthermore, a couple of O（7）–H（10）？？？O（3） hydrogen bonds were formed by O atom of P=O and H atom from hydroxyl in the solvent ethanol. Thermal property of the compound was also studied by means of thermogravimetry （TGA）. The thermal analysis and preliminary fireproofing test show that the title compound has good flame retardance.展开更多
Keeping in view the biological activities of 1,3,2-dioxaphosphorinane-2-one and oxime esters. some compounds possessing these two moieties have been synthesized. The configurational assignment and the ratio of cis/tra...Keeping in view the biological activities of 1,3,2-dioxaphosphorinane-2-one and oxime esters. some compounds possessing these two moieties have been synthesized. The configurational assignment and the ratio of cis/trans diastereomers of target products were performed on basis of H-1 NMR. P-31 NMR and confirmed by X-ray diffraction analysis.展开更多
基金Supported by the Youth Foundation of Hubei Educational Committee(No.Q20151902)the State Undergraduate Innovative Training Program(No.201410517002)the Start-up Foundation for Doctor of Hubei University for Nationalities(No.MY2013B027)
文摘The title compound, 2-（3-silatranylpropylamino）-4-dichlorophenyl-5,5-dimethyl- 1,3,2-dioxaphosphorinane-2-oxide （2（C20H33N2O6Psi）？C2H6O？CH4O, Mr = 991.20）, has been synthe- sized by the nucleophilic substitution reaction of 2-chloro-4-phenyl-5,5-dimethyl-1,3,2-dioxa- phosphorinane-2-oxide with γ-aminopropylsilatrane, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P with a = 10.3783（15）, b = 11.2402（17）, c = 12.1675（18） ？, ？ = 70.653（4）, ？ = 82.908（4）, ？ = 85.690（4）？, V = 1328.1（3） ？3, Z = 1, Dc = 1.239 g/cm3, μ = 0.19 mm？1, F（000） = 532, the final R = 0.0640 and wR = 0.2090 for 3615 observed reflections with I 〉 2？（I）. The cyclic dioxaphosphorinane ring in the molecule adopts a thermodynamically stable cis conformation, while the silatrane fragment forms a cage-like structure in which there exists an intramolecular Si？N donor-acceptor bond. In the crystal structure, centrosymmetrically related molecules are linked by pairs of N–H？？？O hydrogen bonds into dimers, generating rings with graph-set motif R22（8）. Furthermore, a couple of O（7）–H（10）？？？O（3） hydrogen bonds were formed by O atom of P=O and H atom from hydroxyl in the solvent ethanol. Thermal property of the compound was also studied by means of thermogravimetry （TGA）. The thermal analysis and preliminary fireproofing test show that the title compound has good flame retardance.
文摘Keeping in view the biological activities of 1,3,2-dioxaphosphorinane-2-one and oxime esters. some compounds possessing these two moieties have been synthesized. The configurational assignment and the ratio of cis/trans diastereomers of target products were performed on basis of H-1 NMR. P-31 NMR and confirmed by X-ray diffraction analysis.
