- Investigation of the solubility of octahydro-1,3,5,7-tetranitro-1,3,5,7- tetrazocine and 1,3,5-triacetyl-hexahydro-s-triazine
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Octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (TAT) was produced by condensation of acetonitrile and trioxane as a low cost precursor for the production of 1,3,5,7-tetranitro-octahydro-1,3,5,7-tetrazocine (HMX). However, 1,3,5-triacetyl-hexahydro-s-triazine (TRAT) was also produced as a byproduct. To develop an efficient and economical method for the separation of TAT and TRAT, the solubilities of TAT and TRAT in ethyl acetate, methanol, acetonitrile and deionized water were investigated at temperatures between 298 K and 318 K. TAT was found to be relative insoluble in ethyl acetate with a maximum solubility of about 0.0295 mol/kg ethyl acetate at 318 K, which was an order of magnitude lower than that of TRAT (0.371 mol/kg ethyl acetate). TRAT was also relatively insoluble in water (0.712 mol/kg water). Accordingly, a method for the separation of TAT and TRAT based on recrystallization in ethyl acetate and precipitation by deionized water was developed. TAT was recrystallized from ethyl acetate with a purity of 97.9 %, and TRAT was recovered from the ethyl acetate filtrate by addition of water with a purity of 98.9 %.
- Wang, Lei,Xu, Zihibing,Wang, Peng,Wang, Lisheng,Lin, Zhihui,Meng, Zihui
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- Triacylperhydro-1,3,5-triazines over phenylsulfonic acid functionalized mesoporous silica
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An operationally simple, efficient, and environmentally benign synthesis of 1,3,5-triacylperhydro-1,3,5-triazines in good yields by reaction of different organic nitriles and trioxane in the presence of phenylsulfonic acid functionalized mesoporous silica under mild conditions was examined. The yields of the corresponding 1,3,5-trisubstituted perhydro-s-triazines synthesized from acetonitrile, propionitrile, butyronitrile, benzonitrile, and 1.3.5-trioxane were 95.7%, 96.1%, 84.2%, and 98.1%, respectively. The products were characterized by 1H NMR, infrared, mass spectrometry, and elemental analysis. The mechanism of the formation of 1,3,5-triacylperhydro-1,3,5-triazines in acidic conditions was also described using a model reaction of butyronitrile with trioxane.
- Yang, Jianming,Yu, Qinwei,Zhao, Fengwei,Lu, Jian,Ge, Zhongxue
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- Synthesis of 1,3,5-Triacylperhydro-1,3,5-triazines Catalyzed by Ion-Exchange Resins
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1,3,5-Triacylperhydro-1,3,5-triazines can be obtained in high yields by reaction of 1,3,5-trioxan with nitriles in solvents such as chlorobenzene using as catalyst an ion-exchange resin such as Amberlyst 15 with precise control of the hydration rate of the resin.
- Ladhar, F.,El Gharbi, R.,Delmas, M.,Gaset, A.
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- Reactions of amidosulfuric acid salts with formaldehyde
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Potassium amidosulfate reacts with formaldehyde at pH 7-12 to afford a mixture of dipotassium 4-hydroxy-1,3-diazabutane-1,3-disulfonate hydrate and tripotassium 6-hydroxy-1,3,5-triazahexane-1,3,5-trisulfonate HO(CH2NSO3K)n·H2O (n = 2, 3). The reaction of the same compounds at pH 1-3 gives diammonium 1,3,5,7-tetraazabicyclo[3.3.1]nonane-3,7-disulfonic acid sulfate dihydrate.
- Lyushnina,Bryukhanov,Turkina,Malakhov,Golod
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p. 1030 - 1033
(2007/10/03)
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- Preparation of hexahydro-1,3,5-trialkanoyl-s-triazines
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Hexahydro-1,3,5-trialkanoyl-s-triazines are produced by reacting a polymeric formaldehyde and an alkanoic acid amide in the presence of sulfuric acid catalyst and a liquid organic solvent or diluent while removing the water formed in the reaction by distillation, the amount of sulfuric acid catalyst employed being at least 0.05 mol per mol of said amide.
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