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设计合成了5种新型烷基取代酰肼-吡啶-N-氧化物,并将其作为水相铜催化含氮杂环与芳香碘代物偶联反应的配体.实验结果表明,十二烷基取代酰肼-吡啶-N-氧化物的催化效果最佳.对影响反应的其它条件,如铜源、碱、反应时间和温度等条件进行了优化,建立了最佳反应条件:CuO(10%,摩尔分数),NaOH(1 mmol),TBAB(5%,摩尔分数),L5(20%,摩尔分数),于120℃反应12 h,无需惰性气体保护.在此条件下,芳香碘代物与咪唑偶联反应的产率为60%~92%.该方法的特点是以水作为反应溶剂,长链烷基取代酰肼-吡啶-N-氧化物同时起到了铜催化剂配体和相转移催化剂的作用. 相似文献
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以聚苯乙烯-二乙烯苯接枝磷钨酸季铵盐为三相相转移催化剂,以H2O2为氧化剂,KCl为助催化剂,研究了环戊烯(CPE)合成环氧环戊烷(CPEO)的无溶剂工艺。 讨论了催化剂和助催化剂用量、反应温度、反应时间、环戊烯与H2O2摩尔比对反应的影响。 确定了无溶剂环氧环戊烷合成反应的条件为(以0.056 mol H2O2计):催化剂1.0 g、助催化剂0.025 g、反应温度40 ℃、反应时间5 h、n(CPE)∶n(H2O2)=2.1∶1.0。 CPEO的平均收率约为96%。 催化剂回收重复使用6次活性无明显降低。 相似文献
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研究了Fe(Ⅲ)催化氯代炔烃水化生成α-氯代甲基酮化合物的反应,考察了催化剂的种类、酸的种类、反应温度以及溶剂对反应的影响.结果表明,采用Fe Cl3·6H2O(摩尔分数5%)和甲基磺酸(摩尔分数20%),在1,2-二氯乙烷溶剂中,氯代炔烃于80℃进行水化反应3 h,可以高产率得到α-氯代甲基酮产物.所得化合物的结构采用IR,1H NMR,13C NMR及MS等方法进行了表征.该水化反应合成方法简单、条件温和且收率良好,为合成α-氯代甲基酮提供了一种简便途径. 相似文献
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以固体超强酸SO2-4/ZrO2-Fe2O3催化合成醋酸异戊酯 总被引:3,自引:0,他引:3
以合成醋酸异戊酯为探针反应,筛选出制备固体超强酸SO2-4/ZrO2-Fe2O3(SZF-1)的最佳工艺条件为ZrOCl2·8H2O 9.7 g, FeCl3·6H2O 16.2 g, 常温陈化24 h, 0.5 mol·L-1 H2SO4(15 mL·g-1)浸泡5 h, 550 ℃焙烧3 h.以SZF-1为催化剂合成醋酸异戊酯的反应条件为异戊醇200 mmol, n(异戊醇)n(醋酸)=1.0 1.3, SZF-1 1 g(反应物总质量的3%), 环己烷15 mL, 回流反应3 h, 酯化率93.47%.催化剂连续使用6次后酯化率仍在70%以上. 相似文献
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利用三缺位Keggin型杂多酸[A-α-PW9O34]9-和[(FeШ(OH2)2)3(A-α-PW9O34)2]9-的四丁基铵盐做为催化剂,H2O2做为氧化剂催化环己烯氧化反应. 考察了反应时间、H2O2与环己烯的摩尔比,催化剂的用量等因素对反应结果的影响. 结果表明:在1, 2-二氯乙烷为10 mL,H2O2 (30 %)与环己烯的摩尔比为2,反应温度为35 oC,反应时间为6 h,[(C4H9)4N]9[A-α-PW9O34]为催化剂的条件下,环己烯氧化反应的转化率为55 %,主要产物是环氧环己烷,其选择性 ≥ 99 %;而以[(C4H9)4N]9[(FeШ(OH2)2)3(A-α-PW9O34)2]为催化剂时环己烯氧化反应的转化率17 %,主要产物是2-环己烯-1-酮,选择性 ≥ 99 %. 相似文献
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采用水热法添加模板剂十六烷基三甲基溴化铵(CTAB)和配合剂柠檬酸(CA)制备了Mo VTe Nb O系列催化剂,并将其应用于丙烯一步氧化制备丙烯酸的反应.结果表明,CA的添加量对催化剂的形貌、孔结构、比表面积及催化性能具有明显的影响.当n(CA)/n(Mo)=0.36时,Mo VTe Nb O催化剂为介孔纳米催化剂,其平均孔径为4.9 nm,具有较高的比表面积(37.8 m2/g)和较小的催化剂晶粒(粒径范围为10~16 nm),与常规水热法制备的催化剂相比,Mo VTe Nb O介孔纳米催化剂的晶粒变小、催化性能得到了显著提高,丙烯一步氧化制丙烯酸的转化率可由53.9%提高至71.2%,丙烯酸收率可提高到45.8%. 相似文献
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A new complex (1) was prepared by mixing pyridinium polystyrylsulfonate resin and aqueous fluoboric acid, followed by being dehydrated. 1 can be used as an acidic catalyst for the acetalization of benzaldehyde with n-butanol with a highly catalytic activity. The characterization and reusability of 1 are discussed. 相似文献
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V. G. Vasil’ev L. A. Wasserman G. G. Nikiforova L. I. Komarova G. I. Timofeeva I. G. Plashchina S. N. Salazkin V. S. Papkov 《Polymer Science Series A》2014,56(1):17-25
New derivatives of polydiphenylenesulfophthalide, namely its alkali-metal salts and interpolymer complexes with a cationic surfactant, are prepared via polymer-analogous transformations. It is shown that, depending on the type of solvent, solutions of polydiphenylenesulfophthalide salts may feature the properties of polyelectrolytes or ionomers. On the basis of dynamic laser light scattering data, the sizes of associates formed in solutions of salts of polydiphenylenesulfophthalide and its complexes with cetyl pyridinium chloride are determined. With the use of dynamic drop tensiometry, the values of surface tension of the aqueous solutions of lithium polydiphenylenesulfophthalide and its complexes with cetyl pyridinium chloride, as well as viscoelastic characteristics of adsorption layers formed at the solution/air interface, are measured. 相似文献
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We prepared test solutions which contained 80% (v/v) ethanol and 0.2% (w/v) chlorhexidine (CH) or benzalkonium chloride (BC) with or without a dibasic acid diester. After complete evaporation of the ethanol from the solution on filter paper, an overnight broth culture (Staphylococcus aureus) was repeatedly inoculated onto the filter paper, and viable bacterial counts were measured at 5 min after the last inoculation. By comparison with viable counts for CH or BC alone, we estimated the potentiating effects of dibasic acid diester on the bactericidal activity of CH or BC, and confirmed that this activity of the two disinfectants was potentiated in the presence of certain compounds in the homologs of di-n-butyl esters of aliphatic dibasic acid, and di-alkyl esters of adipic and phthalic acid. Diisobutyl adipate, one of the most effective diesters, substantially enhanced the bactericidal activities of benzethonium chloride, cetyl pyridinium chloride and didecyl dimethyl ammonium chloride, as well as CH and BC, but not those of polyhexamethylene biguanide or alkyldiaminoethyl glycinate. The potentiating effects of dibasic acid diesters observed for both CH and BC seemed to be affected by the hydrophobic character of these diesters themselves and are also expressed well by a particular quadratic equation as a function of these characters: namely, capacity factors, as determined by high-performance liquid chromatography. 相似文献
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Methyl 2-substituted-4-benzoxazolecarboxylates were synthesized from methyl 2-amino-3-hydroxybenzoate and the corresponding acid chloride or ortho acetal with pyridinium p-toluenesulfonate as an acid catalyst. Decomposition due to hydration at the 2-position was seen for some compounds during purification. 相似文献
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E. A. Dikusar N. I. Nechai V. I. Potkin R. V. Kaberdin N. G. Kozlov N. V. Kovganko 《Chemistry of Natural Compounds》2003,39(2):186-190
Previously unknown esters 1b-14b were prepared by reaction of cetyl alcohol 1a, terpene alcohols 2a-6a, sterols 7a-11a, and plant phenols 12a-14a with 4,5-dichloroisothiazol-3-carboxylic acid chloride. 相似文献
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E. A. Dikusar N. G. Kozlov V. I. Potkin N. V. Kovganko 《Chemistry of Natural Compounds》2003,39(3):276-279
Esters 1b-15b were prepared from cetyl alcohol 1a, terpenols 2a-6a, sterols 7a-10a, plant phenols 11a-13a, and alcohols 14a-15a by reaction with 1-adamantanecarboxylic acid chloride in the presence of pyridine. 相似文献
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E. A. Dikusar V. I. Potkin S. K. Petkevich R. V. Kaberdin N. G. Kozlov A. V. Bazhanov N. V. Kovganko 《Chemistry of Natural Compounds》2004,40(3):230-234
Previously unknown (Z)-3,4,4,4-tetrachlorobut-2-enoates 1b-20b were prepared in 77-88% yields by reaction in the presence of pyridine of 3,3,4,4,4-pentachlorobutanoic acid chloride with cetyl alcohol (1a), terpenols and terpenone oximes (2a-13a), sterols (14a and 15a), diosgenin (16a), and plant phenols and their oximes (17a-20a). 相似文献
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以聚乙烯醇和单宁酸为原料制备出了形状记忆水凝胶,以乙二胺四乙酸、二水合氯化铜、六水合氯化镁、氧化铝为原料制备出了无机热致变色材料,以结晶紫内酯、硼酸、十六醇为原料制备出了有机热致变色材料,并将形状记忆材料与热致变色材料结合,成功制备出了两种既能记忆形状又能变色的新型复合高分子材料。本实验原料简单易得,方法简便,并与本科阶段有机化学、无机化学、仪器分析、精细化学品化学等课程中所学习的自由基聚合反应、化学交联、络合反应等知识结合,可作为本科教学的一个综合实验,提高学生的动手能力,激发学生学习化学的兴趣和热情。 相似文献