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二甲基对溴碘代苯是带有两种不同卤素基团的芳香族有机合成中间体。2,6-二甲基苯胺在过碳酸钠作用下,于45~50℃与碘反应1 h,得到2,6-二甲基-4-碘苯胺,收率42.5%。2,6-二甲基-4-碘苯胺在-5~0℃下进行重氮化,进一步与溴化亚铜发生Sandm eyer反应,得到3,5-二甲基-4-溴碘苯,收率31.5%。2,6-二甲基苯胺室温下与六亚甲基四胺溴络合物反应30 m in,得到2,6-二甲基-4-溴苯胺,收率62.0%。2,6-二甲基-4-溴苯胺在-5~0℃进行重氮化,与K I反应,得到2,6-二甲基-4-溴碘苯,收率33.1%。通过熔点、红外光谱和核磁共振氢谱对中间体2,6-二甲基-4-碘苯胺、2,6-二甲基-4-溴苯胺以及最终产物3,5-二甲基-4-溴碘苯和2,6-二甲基-4-溴碘苯进行了表征。 相似文献
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介绍了经改进的奥美拉唑中间体2-巯基-5-甲氧基-1 H-苯并咪唑的合成工艺。以对甲氧基苯胺为原料,经胺基保护、硝化、水解得到4-甲氧基-2-硝基苯胺,再经Pd/C催化下还原后,直接与CS2缩合成环反应制得奥美拉唑重要中间体2-巯基-5-甲氧基-1 H-苯并咪唑。对实验过程中的硝化反应和催化还原反应的条件进行了探讨。该方法具有反应条件温和、操作简便、环境污染小的特点,适合工业化生产。 相似文献
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《化学工程》2021,49(7)
采用具有脉冲变径结构的微通道反应器,以2,4-二硝基-6-溴苯胺为原料,质量分数40%NOHSO_4为重氮化试剂,连续合成了2,4-二硝基-6-溴苯胺重氮盐。考察了2,4-二硝基-6-溴苯胺摩尔比、反应温度、98%H_2SO_4用量、停留时间等因素对重氮化反应的影响。通过实验确定较优工艺条件为:2,4-二硝基-6-溴苯胺与40%NOHSO_4摩尔比为1∶1.01,98%H_2SO_4用量为2,4-二硝基-6-溴苯胺2倍,反应温度为70℃,停留时间为250 s。该条件下,2,4-二硝基-6-溴苯胺转化率达99.4%,重氮盐选择性达96.9%。与已报道的间歇工艺相比,连续流工艺大幅缩短了反应时间,提高了重氮盐的纯度,具有一定的工业化应用前景。 相似文献
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以2-甲基-6-硝基苯胺为起始物,氨基重氮化后转化为氰基,然后氰基水解成羧基,最后以硫化钠作还原剂,将硝基还原成氨基得到2-氨基-6-甲基苯甲酸,总收率为38.1%。重氮化反应中2-甲基-6-硝基苯胺与盐酸的最佳摩尔比为1∶2.2,Sandmeyer氰化在室温反应3h后,升温至60°C反应30min收率最佳。 相似文献
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(E)-6-碘-3-(2-(吡啶-2-基)乙烯基)-1-(四氢-2 H-吡喃-2-基)-1 H-吲唑是阿西替尼的关键中间体,以6-硝基-1 H-吲唑为起始原料,经过碘代、加成、偶联、还原、碘代得到目标化合物。探讨了用微波辐射加热偶联反应的问题,并对各步反应合成条件进行了优化。改进后工艺总收率达42.32%(6-硝基-1 H-吲唑为原料计),收率比文献报道值提高近5%,目标化合物和各中间体经1 H NMR和MS等确证结构。改进后的工艺降低了成本,简单可行,适合工业化生产。 相似文献
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以亚磷酸三乙酯与氯化苄或对甲基氯化苄反应制备W ittig试剂,再与N,N-二(甲)苯基氨基苯甲醛反应,高收率制备了N,N-二(4-甲基苯基)-4-〔2-(4-甲基苯基)乙烯基〕苯胺(Ⅱa)、N,N-二(4-甲基苯基)-4-(2-苯基乙烯基)苯胺(Ⅱb)、N,N-二苯基-4-〔2-(4-甲基苯基)乙烯基〕苯胺(Ⅱc)、N,N-二苯基-4-(2-苯基乙烯基)苯胺(Ⅱd)4种空穴传输材料,收率分别达96.4%、92.1%、89.4%、92.6%。产物通过元素分析、红外光谱和质谱等进行了表征。以Y-TiOPc为电荷产生材料,合成化合物为空穴传输材料,制备了有机光导体,并进行了光电性能测试,化合物Ⅱa、Ⅱb和Ⅱc光敏性均在0.04~0.05 lx.s,是性能优异的电荷传输材料。 相似文献
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本工作合成了一系列带取代基的苯基重氨盐化合物。对它们的直接光解研究表明:带推电子基的重氮盐化合物具有较高的光解反应速度,但在敏化光解研究中发现:带有拉电子基的重氟盐化合物,不论是它的敏化光解或是猝灭敏化剂荧光的能力都较带推电子基的重氮盐为强,这清晰地表明,此敏化过程是通过电子转移反应而实现的。工作中还发现,在基态条件下,重氮盐和N,N-二甲基苯胺间可生成电荷转移络合物(CTC),经Benesi-Hildebrand公式处理表明:可形成1:1的CTC。 相似文献
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《Dyes and Pigments》1986,7(3):215-230
The effect of pH on the diazo coupling reaction of some commonly used coupling components (J-acid, Gamma acid, H-acid and S-acid) with monosubstituted diazobenzenes has been investigated. The results demonstrate that, contrary to previous reports, selective diazo coupling ortho to an amino group of an aminohydroxynaphthalenesulfonic acid does not occur in weakly acidic (pH 5–6) media. In fact, such media were found to give nearly exclusive diazo coupling ortho or para to the hydroxyl group. The desired amine coupling reactions required a pH of 3.0–3.5 and occurred only with the more reactive diazonium salts. The structures of the dyes obtained were unambiguously determined with the aid of 1H-NMR spectroscopy. 相似文献
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Solvent Effects in the Photoinduced Electron Transfer Reaction of Uncharged Donors with Arenediazonium Salts In the photochemical electron transfer reactions to arene diazonium salts no strong Coulomb forces arise but the rate constants possibly vary in dependence on the state of the diazonium salt (tight ion pair in nonpolar solvents or free diazonium cations). This problem is studied in the present work using anthracene and tetracene, respectively, as electron donors. They react in their S1 states diffusion-controlled with ion pairs ArN2⊖ BF4⊖, whereas the respective triplet reactions proceed up to 103 times more slowly. These rates are not significantly influenced by the dielectric properties of the solvent. Thus, ion pairing of the diazonium salts in solvents of low polarity has no screening effect on the electron transfer. This behavior is explained including electrostatic effects into the MARCUS theory of outer sphere electron transfer processes. No indication of a Marcus inverted region was found. 相似文献
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《Journal of Sulfur Chemistry》2013,34(1):63-85
Syntheses and reactions of 2-amino-4-substituted-1,3-thiazoles are reviewed in a formal way. The title compounds are most easily accessible by various approaches, and even waste-free solid-state procedures have been developed. The substitution in 4-position has synthetic reasons and therefore most interest accumulates around these derivatives of 2-aminothiazole. The high reactivity of both the amino group and the positions 3 and 5 of the 1,3-thiazole ring are used for numerous syntheses in a comprehensive way. The reactions are subdivided in groups that cover reactions at the amino substituent without touching the thiazole ring, reactions which involve both nitrogens in the formal amidine system to give thiazolo-pyrimidinones and -imidazoles as well as more involved polycondensed N,S-heterocycles with multiple possibilities for substituents, and substitution reactions at the 5-position of the thiazole ring. Most of the imaginable reaction types have been successfully applied and used, as many of the synthesized compounds exhibit interesting biological activity in various fields. 相似文献
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Light Absorption and Substituent Effects of Stibene-4-diazonium Ions Substituent effects on ṽmax-values of 31 stilbene-4-diazonium ions are studied. With increasing donor strength of a substituent in 4′-position the long wave absorption band of stibene-4-diazonium ions shifts from the ultraviolet to the red region of the spectrum. The particular deep colour of diazonium compounds may be described by the very high σp-Hammett-constant of the diazonium group. The substituent effects found characterize stilbene diazonium ions as typical donor-acceptor chromogenes. 相似文献