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含能材料  2009 

1,4-二硝基呋咱并[3,4-b]哌嗪(DNFP)的合成

DOI: 10.3969/j.issn.1006-9941.2009.05.010

Keywords: 有机化学,1,4-二硝基呋咱并[3,4-b]哌嗪(DNFP),呋咱,哌嗪,合成,表征

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Abstract:

设计合成了高能量密度材料1,4-二硝基呋咱并[3,4-b]哌嗪(DNFP)。即以N,N′-二叔丁基乙二胺为起始原料,低温条件下与二氯乙二肟缩合环化生成1,4-二叔丁基哌嗪-2,3-二酮肟(PDO-tB),而后在氢氧化钠的乙二醇溶液中高温反应脱水环化得1,4-二叔丁基呋咱并[3,4-b]哌嗪,经98%硝酸和硫酸的混酸体系硝解合成出DNFP,总收率32.6%,采用红外光谱、核磁共振谱、元素分析对DNFP和中间体结构进行了表征;改进了PDO-tB的合成工艺条件,加料方式由一次性加入改为缓慢滴加,并确定了适宜的冷浴温度为-18℃;研究了不同硝解体系对反应的影响,确定了适宜的硝解体系为硝硫混酸,硝解收率为61.7%。

References

[1]  Cichra D A,Holden J R, Dickinson C. Estimation of normal densities of explosives from empirical atomic volumes [R]. NSWC Report TR79-273,1980.
[2]  Rothstein L R,Petersen R. Predicting high explosive detonation velocities from their composition and structure[J]. Prop and Explo, 1979, 4:56-60.
[3]  Rothstein L R. Predicting high explosive detonation velocities from their composition and structure[J]. Prop and Explo, 1981,6 : 91 - 93.
[4]  Ronald A. Advanced Energetic Materials[M]. Washington D C: National Academies Press ,2004.
[5]  Fried Laurence E, Manaa M Biad,Pagoria Philip F,et al. Design and synthesis of energetic materials [J]. Annual Review of Materials Research,2001,31 : 291 -321.
[6]  Rodney L Willer, Donald W Moore. Synthesis and chemistry of some furazano- and furoxano [ 3,4-b ] piperazines [J]. J Org Chem, 1985, 50:5123 -5127.
[7]  Rodney L Wilier, Ridgecrest Calif. Synthesis of 1,4-dinitrofurazano [ 3,4-b ] piperazine : USP 4539405 [P] , 1985.
[8]  Oyumi Y,Rheingold A L,Bfill T B. Thermal decomposition of energetic materials. 16. solid-phase structural analysis and the thermolysis of 1,4-dinitrofurazano[ 3,4-b ] piperazine [J]. J Phys Chem, 1986,90 :4686 - 4690.
[9]  Oyumi Y, Brill T B. Thermal Decomposition of energetic materials 22.the contrasting effects of pressure on the high-rate thermolysis of 34 energetic compounds [J]. Combustion and Flame, 1987,68 : 209 - 216.
[10]  Oyumi Y, Brill T B. Thermal decomposition of energetic materials.23. thermochemical differentiation of cyclic and acyclic nitramines by their phase transitions [J]. Thermochimica Acta, 1987 ,116 : 125 - 130.
[11]  Patil D G, Brill T B. The thermal decomposition of energetic materials.Part 64. kinetics of decomposition of furazano[ 3,4-b] piperazine and its 1,4-dinitro nitramine derivative [J]. Thermochimica Acta, 1994, 235 : 225 - 230.
[12]  Haaf Michael,Schmedake Thomas A,Paradise Bryan J,et al. Synthesis and reactivity of the stable silylene N, N\\'-di-tert-butyl-1,3-diaza-2- sila-2-ylidene[J]. Can J Chem,2000,75 : 1526 - 1533.
[13]  黄明(HuangM) 李洪珍(LiHZ) 李金山(LiJS).[J].含能材料,2006,14(2):114-115.
[14]  Adolph Horst G. Fluoronitroaliphatics. VI. Preparation of N-(2,2,2-fluorodinitroethyl) - amides [J]. J Org Chem, 1972,37 ( 5 ) : 747 - 751.
[15]  Cilligan William H. Synthesis of N,N-bis(2-fluoro-2,2-dinitroethyl)-N-alkylamines[J]. J Org Chem,1971,36(15) : 2138 -2141.
[16]  Cichra Dorothy A, Adolph Horst G. Nitrolysls of dialkyl tert-butylamines[J]. J Org Chem,1982,47:2474 -2476.

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