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在完全除去铵离子的湿法氧化反应中,一种钌催化剂能够将文献报道的反应条件从543K,7.0 MPa缓和为453 K,3.0 MPa.但是,在相对温和的反应条件下,N2选择性不够理想,并受到操作条件如pH、反应温度、空填充压力及催化剂用量等的影响.在所试验的条件范围内,N2选择性在85.6%~98.1%间变化,而氨转化率却接近100%.对N2选择性和反应条件之间的关系进行了讨论,并通过正交试验找到了一个最佳反应条件,从而在温和的反应条件下,使氨的氧化能够有效地向着生成N2的方向进行. 相似文献
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Yasunori Sudoh Zhong-Tian Jin Kimiaki Imafuku Hisashi Matsumura 《Journal of heterocyclic chemistry》1982,19(3):525-528
The reaction of 3-acetyltropolone ( 1 ) with hydroxylamine under the acidic condition gave 3-methyl-8H-cyclohept[d]isoxazol-8-one ( 4 ) and its oxime ( 5 ), and under the neutral condition gave 4 and 3-acetyltropolone oxime ( 6 ). The reaction of 3-acetyl-2-methoxytropone ( 2a ) with hydroxylamine under the acidic condition gave 4, 5 , and 4-methyl-1H-2,3-benzoxazin-1-one ( 7 ), and under the neutral condition gave 4, 7 , 3-methyl-8H-cyclohept[c]isoxazol-8-one ( 8 ), and its oxime ( 9 ). The reaction of 7-acetyl-2-methoxytropone ( 2b ) with hydroxylamine under the acidic condition gave 4 and 5 , and under the neutral condition gave 5, 7 , and 9 . 相似文献
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Adam Shih-Yuan Lee Shu-Fang Chu Yu-Ting Chang Shu-Huei Wang 《Tetrahedron letters》2004,45(7):1551-1553
A series of homopropargyl alcohols were synthesized from the reaction mixture of zinc powder, 1,2-diiodoethane, 3-bromo-1-propyne and aldehyde or ketone in anhydrous THF under ultrasound. The homopropargyl alcohols were obtained as the only product in all cases when aldehydes were reacted with 3-bromo-1-propyne under this sonochemical Barbier-type reaction condition. The homopropargyl alcohol was produced as the major product and the low contamination of allenyl alcohol was also obtained when ketone was used as substrate under the reaction condition. 相似文献
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LIN Gui-Chun YANG Zhen-Jun ZHANG Liang-Ren LIU Li ZHANG Li-He 《有机化学》2003,23(Z1):30-31
N1-Trifluoroethyl-4-methoxy-5-chloro-3-pyridazone (4) was synthesized by the substitution reaction of 4methoxy-5-chloro-3-pyridazone (1) with trifluoroethyl trifluoromethanesulfonate (A) at basic condition. In the most of reaction conditions, N1-methyl-4-methoxy-5-chloro-3-pyridazone (2) was obtained as a major by-product, which means that the methyl group in the 4-methoxy shifted to N-1 position inter-molecularly aided by A or trifluoroethyl methanesulfonate (B). We obtained N1-methyl-4-trifluoro-ethoxy-5-chloro-3-pyridazone (3) in the reaction of 1 with B at higher temperature in different solvents with different yield (Table 1 ), which mechanism was shown in Figure 1. When we tried to synthesize 4 in the reaction of 1 with trifluoroethyl toluenesulfonate under basic condition, 6 was obtained (Figure 2). All the detailed mechanisms are undergoing investigated. 相似文献
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Novel and unusual dimerization reaction of α-chloroacetoacetanilide under basic reaction condition to give structurally unique 6-oxa-3-azabicyclo[3.1.0]hexane was described. 相似文献
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采用密度泛函理论计算方法, 在B3LYP/6-311G*水平下, 计算并得到了SiHCl3与H2反应各反应通道上各驻点的构型、振动频率和能量. 结果表明, 在气相中SiHCl3分解的通道d和SiHCl3与H2反应的通道c为竞争反应, 但其均未还原出Si原子, 只有衬底Si参与SiHCl3-H2的反应, Si原子才淀积在Si衬底上. 相似文献
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在无模板和表面活性剂的水热条件下,调节反应参数,可以得到一致的片状六方相β-Co(OH)2和多层片状的β-Co(OH)2微/纳米材料.合适的反应条件下,可以制备一致的结晶性好的单片状六方相β-Co(OH)2.用X射线衍射(XRD)、场发射扫描电镜(FESEM)、透射电镜(TEM)、高分辨透射电镜(HRTEM)以及选区电子衍射(SAED)等对反应产物进行了结构和形貌的表征.结果显示,Co(NO3)2的起始浓度、反应温度及溶液成分(异丙醇的加入)对反应产物的形貌结构有着重要的影响. 相似文献
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Sachin V. Bhilare Amol R. Deorukhkar Nitin B. Darvatkar Meghana S. Rasalkar Manikrao M. Salunkhe 《Journal of molecular catalysis. A, Chemical》2007,270(1-2):123-126
Heteropoly acid tungstophosphoric acid (H3PW12O40) was found to be an excellent catalyst for the synthesis of symmetrical diaryl sulfoxides. The reaction was carried out in various organic solvents or ionic liquids and under solventfree condition. The reaction exhibited better results in terms of the yield and rate under solventfree condition. The catalyst was efficiently recovered from the reaction mixture and reused. The highlighting features of the present protocol are short reaction times, high yields of the products, ambient conditions, and simple workup. 相似文献
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P. M. Gorbovoi G. N. Tulaidan B. D. Grishchuk 《Russian Journal of General Chemistry》2008,78(1):133-135
Arenediazonium tetrafluoroborates reacted with 3-chloro-2-methylpropene in the presence of potassium chloride, bromide, and thiocyanate to give the corresponding 1-aryl-3-chloro-2-halo(thiocyanato)-2-methylpropanes. The presence of a copper salt is a necessary condition for the reaction to occur. The yields of the corresponding 1-aryl-3-chloro-2-halo-2-methylpropanes in the Meerwein reaction were approximately twice as low. Introduction of a methyl group to C2 in the 3-chloropropene molecule does not change the reaction regioselectivity. 相似文献
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3,4-Dihydropyrimidin-2(1H)-ones and 3,4-dihydropyrimidin-2(1H)-thione were synthesized under solvent free condition in the presence of nano-silica supported boron trifluoride (nano-BF3.SiO2). The reactions were carried out at 80 °C for 15 min under solvent free condition. This methods have some advantages such as good to excellent yield, mild reaction condition, ease of operation and workup, short reaction time and high product purity. 相似文献
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氨基甲酸酯是合成农药、医药及异氰酸酯的重要中间体^[1,2].传统的氨基甲酸酯的制备是以光气及其衍生物和胺为原料^[3],该工艺使用剧毒的光气,同时副产腐蚀性的HCl.因此,对环境友好的非光气法合成氨基甲酸酯成为当今发展的主流^[4,5].由胺与碳酸二甲酯反应合成氨基甲酸酯是近年发展起来的非光气法,用碳酸二甲酯代替光气合成氨基甲酸酯可以实现环保要求,反应过程中的唯一副产物甲醇可以循环利用.该反应通常在硝酸铅^[6]、γ—Al2O3^[7]、Zn(OAc)2和三氟化镱^[8,9]等催化条件下进行.但上述催化剂存在催化活性低, 相似文献
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Introduction2 Substituted benzothiazolesandtheirderivativeshaveattractedmuchattentionofchemistsandpharmacolo gistsbecauseoftheirbroadspectrumofbiologicalactivi tiesandusesasphotographicmaterials .1 3 Using 2 ben zothiazolylthioacetylhydrazide (1)asabetterrea… 相似文献
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Boric acid (BO3H3) is an inexpensive, efficient and mild catalyst for the synthesis of 1,1-diacetate (acylal) from the various aromatic and heteroaryl aldehydes with acetic anhydride at room temperature under solvent-free condition. The present method does not involve any hazardous organic solvents or catalysts. This method gives notable advantages such as excellent chemoselectivity, mild reaction condition, short reaction times and excellent yield. 相似文献
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在酸碱性条件下对叶绿素-a (1)进行空气氧化反应, 分别得到卟吩衍生物2b~4b; 通过酯交换和去金属镁离子, 将叶绿素-a转化为脱镁叶绿酸-a甲酯(MPa) (5), 其3-位碳碳双键与氯化氢的加成生成卟吩醇(6), 经碱性空气氧化和E-环重排则转化成紫红素-18衍生物7. 选用四氧化锇和高碘酸钠将5氧化成卟吩醛(8), 在丁醇中以丁醇钠作催化剂, 8的氧化和重排反应给出3-甲酰基紫红素-18酯(9)和紫红素-7三甲酯衍生物10. 异构体4的空气氧化和重排反应也生成紫红素-18酯(3), 进一步与2-甲基丁胺进行缩合反应, 得到N-烷基紫红素-18酰亚胺(11a)以及氧化重排产物3-甲酰基-N-烷基紫红素-18酰亚胺(11b). 所得叶绿素衍生物均经UV, IR, 1H NMR及元素分析证明其结构, 并对相应的反应提出可能的反应机理. 相似文献