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四氮烷

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Through the coupling of cyclen and homoserine deriva-tive, we have firstly synthesized a cyclen-functionalized ?α-amino acid,-2-amino-4[1 (1, 4, 7, 10 –tetraazacyclo-dodecane)] butanoic acid.

我们通过1,4,7,10-四氮杂十二烷与高丝氨酸衍生物反应,首先合成了一个非天然α-氨基酸:-2-氨基-4[1(1,4,7,10-四氮杂环十二烷)]丁酸。

Through using Mythylene DinitrAmine as rude product, the knowledge of its reaction properties in different phases have been increased, Through using Mythylene BisAcetAmide as rude product, intermediates which include 1,3-Diacetyl -4,5-dihydroxy -1,3-diazacyclopentane and 1,3-Diacetyl- 4,5-diacetoxy-l,3-diaza cyclopentane have been obtained. 2,4,6,8-tetracetyl- 2,4,6,8-tetraaza bicyclo[3,3,0]octane which can be used to produce Bicyclo-HMX by nitrolysis was also produced. Through using Mythylene BisFormAmide as rude product, intermediates which include 1,3-Diformyl-4,5-dihydroxy- 1,3-diazacyclopentane and 1,3-Diformyl- 4,5-diacetoxy-l,3-diazacyclopentane have been abtained.

以亚甲基二硝胺为初始原料,加深了对亚甲基二硝胺在不同反应相反应特征的认识;以亚甲基二乙酰胺为初始原料,制备了中间体1,3-二乙酰基-4,5-二羟基-1,3-二氮杂环戊烷和1,3-二乙酰基-4,5-二乙酰氧基-1,3-二氮杂环戊烷,最终制备了可被直接硝解为双环HMX的2,4,6,8-四乙酰基-2,4,6,8-四氮杂双环[3,3,0]辛烷;以亚甲基二甲酰胺为初始原料,制备了中间体1,3-二甲酰基-4,5-二羟基-1,3-二氮杂环戊烷和1,3-二甲酰基-4,5-二乙酰氧基-1,3-二氮杂环戊烷。

Major procurement of goods: a three-chlorosilanes, dichloromethane, AE activity ester, 3-iodine Silane, special acid, pentyl chloride, triethylamine, thiadiazole, tetrazolylazo acid, 2 - Acetamide, tetrahydrofuran, the four-guanidine, isopropanol, five phosphorus trichloride, sodium vary bitter, acid, sodium phenylacetate, 6-2 silicon n-amine, Ethylacetoacetate , Methyl isobutyl ketone, potassium dihydrogen phosphate, aluminium oxide, DL methionine, N, N-dimethylaniline, NN-diethyl aniline, 4 sodium EDTA, Anhydrous sodium sulfate, ammonium sulfate, potassium sulfate, sodium acetate, sodium carbonate, DMC, formic acid, sodium chloride medicinal, oxalate, protopine, acetone, alcohol, acetic acid, vinegar Ethyl, butyl acetate, methanol, ethanol (anhydrous, industrial, medicinal), formaldehyde, Ye Jian (30%), hydrochloride (industrial-grade, refined grade, reagent level), sulfate (98%), Ammonia, calcium carbonate, chlorine dioxide, 6 - APA ,7-ACA ,7-ADCA ,7-ANCA, sulbactam, ceftazidime activity ester, Deng salt (hydroxymethyl-K, acid precursors Potassium, sodium dihydrogen methyl), resin, the enzyme, water treatment agent, Xiao Mo agent, demulsifier, flocculants, activated carbon, all kinds of medicinal materials, All kinds of additives

三甲基一氯硅烷、二氯甲烷、AE活性酯、三甲基碘硅烷、特戊酸、特戊酰氯、三乙胺、噻二唑、四氮唑乙酸、二甲基乙酰胺、四氢呋喃、四甲基胍、异丙醇、五氯化磷、异辛酸钠、苯乙酸、苯乙酸钠、六甲基二硅胺烷、乙酰乙酸乙酯、甲基异丁酮、磷酸二氢钾、三氧化二铝、DL蛋氨酸、N,N-二甲基苯胺、NN-二乙基苯胺、乙二胺四乙酸四钠、无水硫酸钠、硫酸铵、硫酸钾、醋酸钠、碳酸钠、碳酸二甲酯、甲酸、药用氯化钠、草酸、片碱、丙酮、正丁醇、冰醋酸、醋酸乙酯、醋酸丁酯、甲醇、乙醇、甲醛、液碱(30%)、盐酸(工业级、精制级、试剂级)、硫酸(98%)、氨水、碳酸钙、二氧化氯、6-APA、7-ACA、7-ADCA 、7-ANCA、舒巴坦、头孢他啶活性酯、邓盐(羟甲基钾、前体酸钾、二氢甲基钠)、树脂、生物酶、水处理剂、消沫剂、破乳剂、絮凝剂、活性碳、各种药用辅料、各种添加剂

The reaction of condensation-cyclization of the two prepared compounds at 100 ℃ in the presence of anhydrous potassium carbonate gave 1,4,7,10-tetrakis(p-toluenesulfonyl)-1,4,7,10-tetraazacyclododecane,with a yield of 71%.

在无水碳酸钾存在下,100℃加热使所得两种磺酰化产物缩合环化得到1,4,7,10-四-1,4,7,10-四氮杂环十二烷,产率71.0%。

Thermal decomposition of octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine in condensed state heated with 5 ℃min^(-1), 10 ℃min^(-1), 20 ℃min^(-1) and 40 ℃min^(-1), respectively, was investigated by in-situ FTIR spectroscope.

采用原位红外光谱研究了炸药1,3,5,7-四硝基-1,3,5,7-四氮杂环辛烷在5,10,20,40℃min^(-1)四种不同升温速率下的热分解行为。

The possibility of synthesizing 2,4,6,8-tetranitro- 2,4,6,8 -tetraazabicyclo[3,3,0]octane(Bicyclo Octogen or Bicyclo- HMX) have been studied.

本文探索了合成2,4,6,8-四硝基-2,4,6,8-四氮杂双环[3,3,0]辛烷的可行性。

In the fifth chapter, six compounds formed between nitrogen-containing ligands such as 2, 2'-bipyridyl, isonicotinamide and 1, 4, 8, 11-tetraazacyclotetradecane and the solution cadmium sulfonates such as 1, 5-naphthalenedisulfonate, 2, 6-naphthalenedisulfonate, 4, 4'-bipenyldisulfonate and 4, 4'-penyletherdisulfonate have been synthesized and structurally characterized. Besides, another compound has been synthesized with cadmium carbonate reacting with 1, 5-naphthalenedisulfonate acid.

第五章以2,2'-联吡啶、异烟酰胺和1,4,8,11-四氮杂环十四癸烷与含有Cd〓和1,5-萘二磺酸根离子、2,6-萘二磺酸根离子、4,4'-联苯二磺酸根离子和4,4'-苯醚二磺酸根离子的水溶液反应,合成了六个化合物,另外以1,5-萘二磺酸与碳酸镉反应合成出一个化合物。

The results show that:(1) When Cu〓 equatorially coordinated by four nitrogen atoms from amine ligands such as ethylenediamine, N-methylethylenediamine, 1, 2-diaminopropane and 1, 4, 8, 11-tetraazacyclotetradecane, etc., Cu〓 could be axially coordinated by oxygen atoms of-SO〓 group.

研究结果表明:(1)当Cu〓在赤道平面与来自胺配体(如乙二胺、N-甲基乙二胺、1,2-丙二胺和1,4,8,11-四氮杂环十四癸烷等)的四个氮原子配位后,在轴向则可以与来自磺酸根离子的-SO〓基团氧原子配位。

Bis-imidazoline was prepared from triethylene tetraamine and N,N-dimethylformamide dimethyl acetal at 85℃ for 2 h with toluene as solvent, with a yield of 90.4%. The reaction of bis-imidazoline with 1,2-dibromoethane and potassium carbonate in acetonitrile provided with a monobromide salt yield of 78.7%. Hydrolysis of monobromide salt under aqueous causic solution formed 1,4,7,10-tetraazzcyclododecane in a 74.2% yield.

用甲苯作溶剂,使三乙烯四胺和N,N-二甲基甲酰胺二甲基缩醛在85℃反应2 h,得到中间体双咪唑啉,产率90.4%,在乙腈溶剂中,碳酸钾存在下,双咪唑啉和1,2-二溴乙烷进行扩环反应,得到环状中间体一溴盐,产率78.7%,一溴盐经碱性水解2 h,得到1,4,7,10-四氮杂十二烷,产率74.2%。

For the above purposes, using a tailored cyanometalate precursor,(1) Tp=hydrotris (pyrazolyl borate; Bu〓N〓=tetrabutylammonium cation , two trinulear complexes,〓(2),〓(3; cyclam: 1, 4, 8, 11-tetraazacyclotetradecane), two one-dimensional polymers,〓(4; dien: diethylenetriamine),〓(5), and a cluster 〓(6) have been synthesized and characterized structurally and magnetically.

基于上述研究热点,我们以修饰的氰基金属化合物(1)为构筑基元(Tp:三吡唑基氢硼烷,Bu〓N〓:四丁基铵离子),合成了两个杂三核化合物,〓(2),〓(3;cyclam:1,4,8,11-四氮环十四烷),两个一维聚合物,〓(4;dien:二乙烯三胺),〓(5),和一个十四核簇合物〓(6)。

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