论文部分内容阅读
The synthetic process for 2,2-dimethyl-5-nitro-5-nitroso-1,3-dioxane(DMNNDO) was improved by using tri(hydroxymethyl)nitromethane and acetone as starting materials through a “one-pot” method combined with alkaline hydrolysis and nitrosation reactions. The yield of DMNNDO was increased from 37% to 45%. The structure of DMNNDO was characterized by IR,~1H NMR,~(13) C NMR,and elemental analysis. Also the thermal decomposition of DMNNDO was studied by using DSC and TG-DTG to find that there are primarily two exothermic decomposition processes between 90 and 300 oC. The crystal structure of DMNNDO was studied by X-ray single-crystal diffraction for the first time. The molecular structure exists as a dimeric form due to the presence of nitroso group. The crystal belongs to monoclinic system,space group C2/c with a = 14.515(3),b = 9.955(2),c = 11.897(2) ?,β = 98.500(3)°,V = 1.6998(2) nm~3,Z = 8,D_c = 1.486 g×cm~(-3),μ = 0.128 mm~(-1),F(000) = 800,S = 1.055,R = 0.0358 and wR = 0.0917. In particular,DMNNDO could be easily hydrolyzed in hydrous systems and the hydrolysis mechanism in CDCl_3 was revealed by means of NMR monitoring.
The synthetic process for 2,2-dimethyl-5-nitro-5-nitroso-1,3-dioxane (DMNNDO) was improved by using tri (hydroxymethyl) nitromethane and acetone as starting materials through a “one-pot” The structure of DMNNDO was characterized by IR, ~ 1H NMR, ~ (13) C NMR, and elemental analysis. The thermal decomposition of DMNNDO was enhanced from 37% to 45% DMNNDO was studied by using DSC and TG-DTG to find that there are both exothermic decomposition processes between 90 and 300 oC. The crystal structure of DMNNDO was studied by X-ray single-crystal diffraction for the first time. The molecular structure exists As a dimeric form due to the presence of nitroso group. space group C2 / c with a = 14.515 (3), b = 9.955 (2), c = 11.897 (3) °, V = 1.6998 (2) nm ~ 3, Z = 8, D_c = 1.486 g × cm -3, μ = 0.128 mm -1, F = 1.055, R = 0.0358 and wR = 0.0917 In particular, DMNNDO could be readily hydrolyzed in hydrous systems and the hydrolysis mechanism in CDCl 3 was revealed by means of NMR monitoring.