共查询到19条相似文献,搜索用时 125 毫秒
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以3,4,5-三氟苯酚、3,5-二氟-4'-烷基联苯为原料,经酚羟基保护反应、丁基锂/碘甲烷上甲基反应、Williamson醚化反应等5步反应最终合成4-[二氟(3,4,5-三氟-2-甲基-苯氧基)甲基]-3,5-二氟-4'-烷基联苯类化合物。纯化后目标产物的气相色谱纯度≥99.5%,总收率约为47%,结构经~1HNMR及GC-MS确证。其中,合成2-(3,4,5-三氟-2-甲基-苯氧基)四氢吡喃适宜的物质的量比为n(2-(3,4,5-三氟苯氧基)四氢吡喃)∶n(丁基锂)=1∶1.2,3,4,5-三氟-2-甲基苯酚和4-溴二氟甲基-3,5-二氟-4'-烷基联苯醚化反应的最优化条件为在DMSO中反应4 h。将该化合物添加到液晶的基础配方中,能降低旋转粘度(γ1),提高液晶的响应速度,增加介电各向异性(Δε),降低阈值电压。 相似文献
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报道了杀菌剂氟嘧菌酯的合成工艺研究。以4-羟基香豆素为原料,依次经过硝化、碱水解、甲胺化、环合、醚化和碱重排环合反应得到(E)-(5,6-二氢-[1,4,2]-二嗪-3-基)-(2-羟基苯基)-甲酮-O-甲基肟(中间体F);以2-氟丙二酸二乙酯为原料,经与醋酸甲脒成环后进行氯化反应合成中间体4,6-二氯-5-氟嘧啶;中间体F先后与4,6-二氯-5-氟嘧啶和2-氯苯酚进行醚化反应得到目标产物氟嘧菌酯。以4-羟基香豆素计,合成总收率达17%,产品质量分数为96%(HPLC)。 相似文献
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[目的]对氟嘧菌酯合成工艺进行清洁化研究。[方法]开发了以4,6-二羟基-5-氟嘧啶为原料,硫酰氟为氟化试剂,“一步法”合成4,5,6-三氟嘧啶的新工艺。4,5,6-三氟嘧啶再与邻氯苯酚和3-[1-(2-羟基苯基)-1-(甲氧亚氨基)-甲基]-5,6-二氢-1,4,2-二嗪经2步醚化反应合成了氟嘧菌酯。[结果]3步反应总收率70.6%,避免了含磷废水排放,并副产氟化钠和氯化钾。[结论]工艺过程清洁、绿色环保、成本低廉,适合工业化生产。 相似文献
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以2,3-二氟苯乙醚和乙酰氯为起始原料,经傅克反应合成了质量分数99%以上的液晶中间体4-乙氧基-2,3-二氟苯乙酮,对目标化合物进行了1HNMR、IR和GC-MS表征。以二氯甲烷为反应溶剂,当n(2,3-二氟苯乙醚)∶n(三氯化铝)∶n(乙酰氯)=1∶1.14∶1.3,反应温度为-10~-5℃,反应时间为1 h时,反应效果最佳,产物质量分数为89.2%,2,3-二氟苯乙醚质量分数为4.83%,副产物4-乙酰基-2,3-二氟苯酚醋酸酯质量分数为0.12%,产物异构体未检出。根据实验结果对傅克反应副产物产生的原因进行了推测。 相似文献
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[目的]合成4,5-二氟-2-羟基苯丁酮并测其农用生物活性。[方法]以3,4-二氟苯酚为原料,与乙酰氯反应成酯以保护酚羟基、以丁酰氯为酰化剂进行傅-克酰基化反应、脱保护得目标产物;以菌丝生长速率法测抑菌活性;以琼脂混药法测除草活性。[结果]产物的1H NMR及质谱分析与目标化合物一致;以无水三氯化铝为催化剂,实施丁酰化过程中可直接得到目标化合物,反应的总收率为67.07%;对苹果腐烂病菌、白菜灰霉病菌、柑橘炭疽病菌的EC50值分别为74.37、100.18、102.77 mg/L;质量浓度为200 mg/L时,对生菜、稗草、反枝苋的根与茎的抑制率均达到60%以上。[结论]以3,4-二氟苯酚为原料进行酚羟基酯化保护,然后以无水三氯化铝为催化剂与正丁酰氯反应不需另外的脱保护过程来制备4,5-二氟-2-羟基苯丁酮是一条高效路线;目标化合物具有较好的抑菌和除草活性。 相似文献
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目前工业化合成硼氢化钠的工艺有Schlesinger法和Bayer法,而Schlesinger法是工业化合成硼氢化钠应用最广的工艺,其关键步骤为氢化钠和硼酸三甲酯的合成。本文一方面从氢化钠的合成、硼酸三甲酯的合成及硼氢化钠的合成3个方面详细论述了Schlesinger法合成工艺进展情况;并指出目前方法存在的问题,如采用油液分散金属钠法合成的氢化钠活性差,制约了氢化钠的应用,硼酸三甲酯工业合成过程中过多使用浓硫酸造成环境严重污染。另一方面对Schlesinger法工艺改进提出了几点设想,如企业全流程合成硼氢化钠可节约外购成本和仓储成本;硼酸三甲酯的合成取代浓硫酸的应用,提纯采用盐析的方法均可以减轻环境污染;硼氢化钠水解过程中采用稀液碱溶液代替淡水,可避免硼氢化钠水解,提高产品收率。 相似文献
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Four commercial polyvinyl alcohol (PVA) and polydimethylsiloxane (PDMS) membranes were applied to the pervaporation of an azeotropic mixture containing trimethyl borate, a precursor to boronic acids used in Suzuki couplings and a gaseous anti‐oxidant in solder flux or brazing. The degree of cross‐linking of the chains in the active layer played a crucial role in the membrane process using the membranes PERVAP 4155‐80, PERVAP 4155‐40 and PERVAP 4155‐30. PERVAP 4155‐30 reached the best results from all tested membranes; an impressive selectivity with fast permeation was also achieved with the PERVAP 4060 membrane. Methanol preferentially passed through PERVAP 4155‐30, but trimethyl borate was favorably pervaporated from the mixture by PERVAP 6040, due to the diverse affinities of the membranes. 相似文献
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Theoretical studies on unsymmetrical electrolyte salts, lithium [1,2-benzenediolato(2-)-O,O′ oxalato]borate (LBDOB), and its derivatives, lithium bis[1,2-benzenediolato(2-)-O,O′]borate (LBBB), and lithium bis(oxalate)borate (LBOB) are carried out using density functional theory (DFT) method and B3LYP theory level. Bidentate structures involving two oxygen atoms are preferred. Based on these conformations, a linear correlation was observed between the highest occupied molecular orbital (HOMO) energies and the limiting oxidation potentials measured by linear sweep voltammetry, which supports experimental results that strongly electron-withdrawing substituent anions are more resistant against oxidation. The correlations were also observed between ionic conductivity and binding energy solubility and theoretical set of parameters of anion, thermal stability and the hardness (η). Wave function analyses have been performed by natural bond orbital (NBO) method to further investigate the cation-anion interactions. 相似文献
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Theoretical studies on a new unsymmetrical electrolyte salt, lithium [3-fluoro-1,2-benzenediolato(2-)-o,o′ oxalato]borate (FLBDOB), and its derivatives, lithium bis[3-fluoro-1,2-benzenediolato(2-)-o,o]borate (FLBBB), and lithium bis(oxalate)borate (LBOB) are carried out using density functional theory (DFT) method and B3LYP theory level. Bidentate structures involving two oxygen atoms are preferred. Based on these conformations, a linear correlation is observed between the highest occupied molecular orbital (HOMO) energies and the limiting oxidation potentials measured by linear sweep voltammetry, which supports experimental results that strongly electron-withdrawing substituent anions are more resistant against oxidation. The correlations are also observed between ionic conductivity and binding energy, solubility and theoretical set of parameters of anion, thermal stability and the hardness (η). Wave function analyses are performed by natural bond orbital (NBO) method to further investigate the cation-anion interactions. 相似文献
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Theoretical studies on unsymmetrical electrolyte salts, lithium difluoro(1,2-benzene-diolato(2-)-o,o′)borate (LDFBDB), and its derivatives, lithium bis[1,2-benzene-diolato(2-)-O,O′]borate (LBBB) and lithium fluoroborate (LiBF4) are carried out using density functional theory (DFT) method and B3LYP theory level. Bidentate structures are preferred. Based on these conformations, a linear correlation was observed between adiabatic ionization potential Ip and the limiting oxidation potentials measured by linear sweep voltammetry, which supports experimental results that strongly electron-withdrawing substituent anions are more resistant against oxidation. The correlations were also observed between ionic conductivity and binding energy, solubility and theoretical set of parameters of anion. Wave function analyses have been performed by natural bond orbital (NBO) method to further investigate the cation–anion interactions. 相似文献