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A Novel Method for Synthesizing 4,4′-Bis(hydroxymethyl)-2,2′-bipyridine
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作者 SU Zhong min CHEN Li hua +3 位作者 WU Li xin XU Hong bin ZHU Dong xia WANG Rong shun 《Chemical Research in Chinese Universities》 SCIE CAS CSCD 2002年第3期345-347,共3页
There are several paths for synthesizing 4,4′ bis(hydroxymethyl) 2,2′ bipyridine, but most of them need strict experimental conditions that are not easy to be overcome. We designed a simple way to prepare this produ... There are several paths for synthesizing 4,4′ bis(hydroxymethyl) 2,2′ bipyridine, but most of them need strict experimental conditions that are not easy to be overcome. We designed a simple way to prepare this product via the oxidation of 4,4′ bismethyl 2,2′ bipyridine, followed by esterification and reduction. The yield increases and the reaction conditions become genial in contrast to those of other methods. The molecular structure of the final product was confirmed by means of elemental analysis, IR, 1H NMR and MS spectra. 展开更多
关键词 4 4-bis(hydroxymethyl)-2 2′-bipyridine Synthesis 4 4-Dimethyl-2 2′-bipyridine
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4,4′-二(羟甲基)联苯的合成、表征与机理探究
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作者 杨涛 唐璇 +2 位作者 薛珊 周宛欣 成西涛 《合成化学》 CAS 2023年第8期580-586,共7页
4,4′-二(羟甲基)联苯是一种重要的化工原料,可用于合成高附加值的有机化合物或新型功能性材料。由于其特殊的结构和性质,4,4′-二(羟甲基)联苯在许多领域都具有广泛的应用和重要性。以4,4′-二(氯甲基)联苯为原料,经水解生成苄醇类化合... 4,4′-二(羟甲基)联苯是一种重要的化工原料,可用于合成高附加值的有机化合物或新型功能性材料。由于其特殊的结构和性质,4,4′-二(羟甲基)联苯在许多领域都具有广泛的应用和重要性。以4,4′-二(氯甲基)联苯为原料,经水解生成苄醇类化合物4,4′-二(羟甲基)联苯。采用1 H NMR,IR和HPLC对产物进行了表征,讨论了溶剂、水解剂、配料比、反应温度、反应时间和催化剂种类对产物含量和收率的影响。优化了4,4′-二(羟甲基)联苯的合成工艺,提出了可能的催化合成反应机理。结果表明:聚乙二醇作为催化剂,可与溶液中的阳离子发生络合,增强了亲核试剂的反应活性,提高了反应速率。在以PEG-600为催化剂,乙腈为溶剂,KOH为水解剂,配料比n(BCMBP)∶n(KOH)=1.0∶3.0,V(乙腈)∶V(H 2 O)=10∶1,78℃反应12 h的优化工艺下,粗产品HPLC含量可达97.2%(质量分数,下同),收率为93.9%。 展开更多
关键词 4 4′-二(氯甲基)联苯 4 4′-二(羟甲基)联苯 合成 表征 催化剂 反应机理 催化酯化
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4,4'-二羟甲基联苯的合成工艺研究 被引量:5
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作者 侯文杰 朱春燕 夏烨 《精细化工原料及中间体》 2009年第10期28-30,共3页
针对4,4'-二氯甲基联苯水解合成4,4'-二羟甲基联苯反应过程,通过对相转移催化法、酯化水解法和溶剂法的比较,选择了溶剂法合成工艺。得到溶剂法合成4,4'-二氯甲基联苯的优化工艺条件,产品收率达到95%以上,经过提纯后产品的... 针对4,4'-二氯甲基联苯水解合成4,4'-二羟甲基联苯反应过程,通过对相转移催化法、酯化水解法和溶剂法的比较,选择了溶剂法合成工艺。得到溶剂法合成4,4'-二氯甲基联苯的优化工艺条件,产品收率达到95%以上,经过提纯后产品的纯度≥98%。 展开更多
关键词 4 4’-二氯甲基联苯4 4’-二羟甲基联苯溶剂法水解
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4,4’-二(氯甲基)联苯在乙腈/水中的水解反应 被引量:5
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作者 来国桥 方奇 +1 位作者 任晓莉 沈永嘉 《高校化学工程学报》 EI CAS CSCD 北大核心 2006年第6期1013-1016,共4页
4,4’-二(氯甲基)联苯在蒸馏水中受热至回流,40h内未观察到有羟基取代苄基中氯原子的亲核取代反应发生。水中有乙腈存在,该反应就会发生,产物是4,4’-二(羟甲基)联苯。反应速度与乙腈/H2O的比例相关,当乙腈/H2O=20/1(容积比)时,完成该... 4,4’-二(氯甲基)联苯在蒸馏水中受热至回流,40h内未观察到有羟基取代苄基中氯原子的亲核取代反应发生。水中有乙腈存在,该反应就会发生,产物是4,4’-二(羟甲基)联苯。反应速度与乙腈/H2O的比例相关,当乙腈/H2O=20/1(容积比)时,完成该反应需要29h;而当乙腈/H2O=1/50时,完成该反应需要46h。若在乙腈/H2O介质中添加KOH,反应速度会加快,但同时会发生副反应以致生成一种淡黄色的树脂状物质。4,4’-二(氯甲基)联苯的纯度高,水解反应的产率及4,4’-二(羟甲基)联苯的纯度也高。当4,4’-二(氯甲基)联苯的纯度从98%降低到92%时,水解反应的产率从98.6%降低到94.4%,产物4,4’-二(羟甲基)联苯纯度从99.2%下降到98.6%。如4,4’-二(氯甲基)联苯的纯度进一步降低到85%,则反应产率急剧下降到80.9%,同时产物4,4’-二(羟甲基)联苯纯度下降到94.3%。 展开更多
关键词 4 4’-二(氯甲基)联苯 亲核取代 水解反应 4 4'-二(羟甲基)联苯
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4,4′-二(羟甲基)联苯合成回收溶剂中二甲亚砜含量的测定方法 被引量:3
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作者 朱春燕 侯文杰 《精细化工中间体》 CAS 2009年第1期65-67,70,共4页
采用高效液相色谱法测定4,4′-二(羟甲基)联苯合成后回收溶剂中二甲亚砜的含量。方法采用ZorbaxSB-C18色谱柱,以甲醇-水(v∶v=13∶7)为流动相,检测波长为210 nm,标准曲线外标法测定回收溶剂中二甲亚砜的含量。二甲亚砜在0.08~0.58mg/m... 采用高效液相色谱法测定4,4′-二(羟甲基)联苯合成后回收溶剂中二甲亚砜的含量。方法采用ZorbaxSB-C18色谱柱,以甲醇-水(v∶v=13∶7)为流动相,检测波长为210 nm,标准曲线外标法测定回收溶剂中二甲亚砜的含量。二甲亚砜在0.08~0.58mg/mL浓度范围内与峰面积呈线性关系,回归方程:y=14.8594x+154.7371,相关系数r=0.99996。平均回收率为100.59%,RSD为0.69%(n=6)。 展开更多
关键词 高效液相色谱 二甲亚砜 4 4′-二(羟甲基)联苯
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4,4'-二羟甲基联苯的提纯工艺研究 被引量:3
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作者 侯文杰 朱春燕 夏烨 《上海化工》 CAS 2010年第8期12-14,共3页
采用对索式萃取、超声提取和溶液结晶等三种分离提纯4,4'-二羟甲基联苯的工艺进行了对比实验,确定了合适的分离提纯工艺,并采用单因素实验优化了分离提纯的工艺条件。结果表明产品的纯度达到99.2%,产品收率81.62%。
关键词 4 4'-二羟甲基联苯 提纯 工艺
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Synthesis, Crystal Structure, and Topology Analysis of One Novel Interpenetrated 2D Cobalt Coordination Polymer, {[Co(HTCB)(4,4'-btb)]·H_2O}_n 被引量:3
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作者 高艳 范黎明 +2 位作者 宋维阔 刘新征 张修堂 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 2014年第9期1333-1338,共6页
One novel cobalt coordination polymer, {[Co(HTCB)(4,4'btb)]'HzO}n (1, H3TCB = 1,3,5-tris(4-carboxyphenyl)benzene, 4,4'-btb = 4,4'-bis(1,2,4-triazol-3-yl)biphenyl), has been synthesized and characterized ... One novel cobalt coordination polymer, {[Co(HTCB)(4,4'btb)]'HzO}n (1, H3TCB = 1,3,5-tris(4-carboxyphenyl)benzene, 4,4'-btb = 4,4'-bis(1,2,4-triazol-3-yl)biphenyl), has been synthesized and characterized by elemental analysis, IR, powder X-ray diffraction (PXRD), and thermogravimetric (TG) analyses. X-ray diffraction analysis reveals that complex 1 is a 2D 2-fold interpenetrated {44,62}-sql [Co(HTCB)(4,4'-btb)] sheet based on the 1D [Co(HTCB)]n chains and 1D [Co(4,4'-btb)]n chains. The crystal of 1 crystallizes in triclinic, space group P1 with a = 9.529(12), b = 13.914(16), c = 14.906(17) A, V= 1903(4) A3, Z = 2, C45H34N6CoO71 Mr= 829.71, Dc = 1.448 g/cm3, F(000) = 858 andμ(MoKa) = 0.514 mm-1. The final R = 0.0655 and wR = 0.1136 for 6603 observed reflections with 1 〉 2a(/) and R = 0.1136 and wR = 0.1747 for all data. 展开更多
关键词 1 3 5-tris(4-carboxyphenyl)benzene 4 4'-bis(1 2 4-triazol-3-yl)biphenyl cobalt interpenetrated topology
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Crystal Structure of an Octanuclear Sandwich Cluster of Silver(I) and 4,4'-Bis(2,5-dimethylstyryl)biphenyl 被引量:1
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作者 刘淑芹 宁桂玲 +2 位作者 张雄福 小中·尚 宗像·惠 《Chinese Journal of Chemistry》 SCIE CAS CSCD 2006年第9期1259-1262,共4页
Reaction of the oligo(phenylenevinylene) 4,4'-bis(2,5-dimethylstyryl)biphenyl (bdb) with CF3CO2Ag in benzene gave a novel octanuclear sandwich cluster [Ags(bdb)2(C6H6)2(CF3CO2)8]·2C6H6 (1). The clu... Reaction of the oligo(phenylenevinylene) 4,4'-bis(2,5-dimethylstyryl)biphenyl (bdb) with CF3CO2Ag in benzene gave a novel octanuclear sandwich cluster [Ags(bdb)2(C6H6)2(CF3CO2)8]·2C6H6 (1). The clusters are packed on each other through strong n-n interactions to form ^1D 'brick' chains, between which the solvated benzene molecules are located. TG analysis showed that cluster 1 could completely liberate the guest benzene molecules at 105℃ and the coordinated benzene molecules at 180 ℃. In solid state, cluster 1 exhibits fluorescence, and the emission band is red-shifted compared with that of free ligand bdb. 展开更多
关键词 silver(Ⅰ) complex octanuclear cluster 4 4'-bis(2 5-dimethylstyryl)biphenyl oligo(phenylenevinylene)
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Enantioseparation of Racemic Anti-hepatitis New Drug Bicyclol with Crystallization 被引量:2
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作者 Wei HU Yan LI Chun Zhen ZHANG 《Chinese Chemical Letters》 SCIE CAS CSCD 2005年第11期1471-1473,共3页
The enantioseparation of anti-hepatitis new drug (±)-bicyclol was performed by optically active alkaloid. The alcoholic acid, the hydrolysate of bicyclol was reacted with optically active alkaloid, such as bruc... The enantioseparation of anti-hepatitis new drug (±)-bicyclol was performed by optically active alkaloid. The alcoholic acid, the hydrolysate of bicyclol was reacted with optically active alkaloid, such as brucine, strychnine, quinidine etc., the diastereoisomeric salts were obtained by fractional recrystallization, then separately decomposed and esterified to obtain the two enantiomers of bicyclol. The pharmacological study showed that the effect of (-)-bicyclol was more potent than racemic bicyclol two times and the potency of (+)-bicyclol was incative. 展开更多
关键词 (±)-bicyclol 4 4'-dimethoxy-2 3 2 3'-bis(methylenedioxy)-6-hydroxymethyl-6'-methoxy-carbonyl biphenyl anti-hepatitis resolution.
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