| 2,3-二羟甲基-2,3-二硝基-1,4-丁二醇四硝酸酯的合成、晶体结构及性能研究 |
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| 引用本文： | 毕福强,姚君亮,王伯周,樊学忠,葛忠学,许诚,刘庆,康冰.2,3-二羟甲基-2,3-二硝基-1,4-丁二醇四硝酸酯的合成、晶体结构及性能研究[J].有机化学,2011,31(11). |
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| 作者姓名： | 毕福强 姚君亮 王伯周 樊学忠 葛忠学 许诚 刘庆 康冰 |
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| 作者单位： | 1. 西安近代化学研究所 西安710065
2. 同济大学化学系 上海200092 |
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| 摘 要： | 以硝基甲烷为起始原料,经缩合、环化、氧化耦合、脱缩酮及硝化等5步反应合成了2,3-二羟甲基-2,3-二硝基-1,4-丁二醇四硝酸酯(BHDBT),总收率为36.1％,并采用核磁共振谱、红外光谱以及元素分析等进行了结构表征.用浓盐酸代替氯化氢气体,改进了关键中间体2,3-二羟甲基-2,3-二硝基-1,4-丁二醇(BHDB)的合成方法,并确定最佳反应条件为:刀(浓盐酸):n(BDND)=1.1∶1,反应温度55℃,时间4h,收率为94.8％.首次发现了BHDB和BHDBT的亚甲基质子具有磁不等价性,并从理论上分析其产生的原因.培养了BHDBT单晶,四元衍射晶体结构解析表明:BHDBT属于单斜晶系,空间群P2(1)/n,晶胞参数:a=0.81944(11) nm,b=2.3365(3) nm,c=0.85838(11) nm,a=90°,β=113.501(2)°,y=90°,V=1.5072(3) nm3,Z=4,Dc=1.852 g·cm-3,μ=0.189 mm-1,F(000)=856.BHDBT熔点为86.37℃,分解峰温度为185.79℃(DSC),摩擦感度为100％ (3.92 MPa,90°),特性落高H50为10.0 cm(5 kg).
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| 关 键 词： | 2 3-二羟甲基-2 3-二硝基-1 4-丁二醇四硝酸酯 合成 晶体结构 性能 |
Synthesis, Crystal structure and Properties of 2,3-Bis(hydroxymethyl)-2,3-dinitro-1,4-butanediol Tetranitrate |
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| Bi, Fuqiang,Yao, Junliang,Wang, Bozhou,Fan, Xuezhong,Ge, Zhongxue,Xu, Cheng,Liu, Qing,Kang, Bing.Synthesis, Crystal structure and Properties of 2,3-Bis(hydroxymethyl)-2,3-dinitro-1,4-butanediol Tetranitrate[J].Chinese Journal of Organic Chemistry,2011,31(11). |
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| Authors: | Bi Fuqiang Yao Junliang Wang Bozhou Fan Xuezhong Ge Zhongxue Xu Cheng Liu Qing Kang Bing |
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| Institution: | Bi,Fuqianga Yao,Junliangb Wang,Bozhou a Fan,Xuezhonga Ge,Zhongxuea Xu,Chenga Liu,Qinga Kang,Binga(a Xi'an Modern Chemistry Research Institute,Xi'an 710065)(b Department of Chemistry,Tongji University,Shanghai 200092) |
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| Abstract: | Starting from nitromethane,2,3-bis(hydroxymethyl)-2,3-dinitro-1,4-butanediol tetranitrate(BHDBT) was synthesized by the condensation,cyclization,oxidative dimerization,deketalization and nitration in total yield of 36.1%.The structures of BHDBT and its intermediates were characterized by means of 1H NMR,13C NMR,FT-IR and elemental analysis.The synthetic process for 2,3-bis(hydroxymethyl)-2,3-dinitro-1,4-butanediol(BHDB) was improved by using concentrated hydrochloric acid instead of HCl gas.It was found tha... |
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| Keywords: | 2 3-bis(hydroxymethyl)-2 3-dinitro-1 4-butanediol tetranitrate synthesis crystal structure property |
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