共查询到19条相似文献,搜索用时 93 毫秒
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采用二氧化硅负载固体磷钨酸盐催化剂,以乙酸酐和噻吩为原料合成2-乙酰噻吩。通过实验考察了固体酸盐催化剂用量、反应时间、反应温度、催化剂重复使用次数对2-乙酰噻吩合成转化率的影响。确定该反应的最适条件为:反应温度85℃,反应时间4h,催化剂用量(质量分数)3.0%-3.5%,催化剂重复使用3次。产品的转化率为80%以上,最高转化率达到90.75%。产品通过气相色谱分析,2.乙酰噻吩质量分数达99.5%以上,副产物主要为3-乙酰噻吩。由此证明,磷钨酸盐作为本反应的催化剂,有着较高的选择性。该方法同以往的方法相比较,具有无设备腐蚀、减少环境污染等优势。产品同催化剂易分离,且催化剂可重复利用。 相似文献
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2-甲基苯并咪唑是重要的医药及染料中间体。以邻苯二胺与乙酸为原料,微波促进001 H型树脂催化合成了2-甲基苯并咪唑。通过单因素实验考察了微波功率、反应时间、原料质量配比、树脂用量、树脂重复使用对2-甲基苯并咪唑合成收率的影响。结果发现,当微波功率为455 W、树脂用量0.5 g、反应时间为30 min、邻苯二胺用量1.08 g、乙酸用量3.24 g时收率最高,可达84.8%。树脂重复使用可行性的研究表明,树脂重复使用两次后,2-甲基苯并咪唑收率从84.8%下降66.7%。结果表明相比于2-甲基苯并咪唑的传统合成方法,具有产率高、工艺操作简单、环境污染效应小等优点,不足之处在于催化剂重复使用性较差,需做进一步的研究工作。 相似文献
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以1-氰乙基-2-甲基咪唑(2MZCN)为原料催化氢化制备1-氨丙基-2-甲基咪唑,考察了反应过程中合成工艺参数对产物的影响,确定较为适宜的工艺条件为:温度100℃,压力5 MPa,转速624 r/min,时间4 h,溶剂是氨的饱和乙醇溶液(与原料质量比是2∶1),雷尼镍为催化剂(占原料质量的18.9%),氢氧化钾为助催化剂,原料的转化率可达99.7%,产率可达94.2%。采用红外光谱(FTIR)和核磁共振氢谱(1HNMR)及气质联用(GC-MS)对产物进行了表征。 相似文献
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A variety of synthetic methods have been developed for azulene derivatives due to their potential applications in pharmaceuticals and organic materials. Particularly, 2H-cyclohepta[b]furan-2-one and its derivatives have been frequently used as promising precursors for the synthesis of azulenes. In this review, we describe the development of the synthesis of azulenes by the reaction of 2H-cyclohepta[b]furan-2-ones with olefins, active methylenes, enamines, and silyl enol ethers as well as their reactivity and properties. 相似文献
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H2SO4-SiO2催化7-羟基-4-甲基香豆素的无溶剂合成 总被引:2,自引:0,他引:2
分别制备了4种H2SO4-SiO2。以H2SO4-SiO2为催化剂,乙酰乙酸乙酯和间苯二酚为原料,通过Pechmann反应,在无溶剂条件下,催化合成了7-羟基-4-甲基香豆素。以4种不同H2SO4-SiO2、催化剂用量、反应时间、反应温度和反应原料的物质的量比设计了五因素四水平的正交试验,得到负载硫酸催化反应的最佳条件:n(H2SO4)∶n(Si)=0.75∶1,n(间苯二酚)∶n(乙酰乙酸乙酯)=1∶1,催化剂用量0.35 g(间苯二酚0.04 mol),反应时间95 min,反应温度105 ℃,最佳条件下产品收率为72.4%。 相似文献
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Anjana Bhattacharya Jagannath Das Swapan Mitra Sisir K. Roy 《Journal of chemical technology and biotechnology (Oxford, Oxfordshire : 1986)》1992,54(4):399-407
Silicoaluminophosphate (SAPO-5) molecular sieves have been synthesised from reaction mixtures having a molar composition of: 0.7–1.0 Al2O3:0.7–1.0 P2O5:0.01–2.0 SiO2:xR:40 H2O (where R = (C2H3)3N or (C2H3)4NOH and x = 1.5–2.5 for (C2H5)5N and 0.5 for (C2H5)4NOH, at 473 K using various sources of alumina and silica. The effects of (i) varying the crystallinity of the alumina source (boehmite) and (ii) the use of different silica sources such as freshly prepared silica either from sodium silicate or paddy husk extract, silica gel from commercial water-glass, and tetraethyl orthosilicate have been studied. The crystallinity of boehmite has been found to have a strong effect on its reactivity towards the formation of SAPO-5. The activity of boehmite for SAPO-5 formation increased with a decrease in its crystallinity (or with increase in its moisture content). Any silica source devoid of sodium ions could be employed for the synthesis of SAPO-5. The process of crystallisation started as early as within 1.5 h of reaction and incorporation of silicon into the AlPO4 framework has been noted at this stage. Formation of some tridymite phase as impurity has been observed under conditions such as (i) SiO2 concentration > 1.7 mole and (ii) x > 2.0 when R = (C2H5)3N. 相似文献