共查询到20条相似文献,搜索用时 125 毫秒
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以3,5二-羟基苯乙酮(4)为原料,经三步反应制得3,5二-乙酰氧基苯乙烯(1)。在硫酸催化下化合物(4)与乙酸酐反应,得到3,5二-乙酰氧基苯乙酮(3),收率92%,对于化合物(3)进行了1H NMR表征;化合物(3)经催化加氢,得到1-(1羟-基乙基)-3,5二-乙酰氧基苯(2),收率98%,对于化合物(2)进行了1H NMR表征;化合物(2)在固体酸催化下反应得到3,5二-乙酰氧基苯乙烯(1),制备化合物(1)的反应条件为:m[化合物(2)]∶m(固体酸)=5∶1,110℃回流5 h,收率95%,纯度98%,对化合物(1)进行了IR,1H NMR,MS表征,并对化合物(1)的1HNMR,MS表征结果进行了进一步分析。 相似文献
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David M. Piatak Kirk A. Ashline George Angelos Rebecca P. Swenson Eliahu Caspi 《Lipids》1982,17(3):235-240
The chemical and spectroscopic properties of several reaction products of 17β-hydroxy-1,3-seco-2-nor-5α-estran-1-oic acid
and 17β-hydroxy-1,3-seco-2-nor-4-oxo-5α-estran-1-oic acid were examined and found to be atypical. For instance, the methyl
ester of the first acid was resistant to basic hydrolysis conditions but partly hydrolyzed with 100% H2SO4. Reduction of the ester by LiA1H4 gave 1,3-seco-2-nor-5α-estrane-1,17β-diol from which diacetate, ditosylate and 17-monotosylate derivatives were prepared.
The C-1 methylene protons of each appeared as a singlet in 60, 100 and/or 270 MHz NMR spectra. The methyl ester and the diacetate
of the diol were synthesized by alternate methods to verify the assigned structures. A 470-MHz spectrum eventually resolved
the C-1 methylene protons of the monotysylate into the AB portion of an ABX pattern, further confirming the assigned structures.
Also, 2,3-seco-1-oxo-5α-estran-17β-ol 17-nitrate was synthesized. 相似文献
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设计了1条以NaHSO4为催化剂合成阿昔洛韦的新工艺,以醋酐和1,3-二氧戊环为起始原料,合成2-氧杂-1,4-丁二醇二乙酯,然后再与乙酰化后的鸟嘌呤发生缩合制得双乙酰阿昔洛韦,双乙酰阿昔洛韦在Na2CO3水溶液中水解得到目标产物阿昔洛韦。考察了该工艺中反应温度、催化剂用量、溶剂等对反应收率和产品质量的影响。结果表明,在合成关键中间体2-氧杂-1,4-丁二醇二乙酯中,反应温度宜选用60℃;合成双乙酰鸟嘌呤时n(鸟嘌呤):n(cat)=1.0:0.1为较佳;合成双乙酰阿昔洛韦时选用甲苯作为反应的较佳溶剂。总收率达到79%,并且产物纯度较高,适合工业化生产。 相似文献
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Summary Copolymers with 2-aceto-1,3-phenanthrenylene units in the chain have been directly prepared by Ru catalyzed step-growth copolymerization of 2-acetyl phenanthrene and ,-dienes such as 1,3-divinyltetramethyldisiloxane. Copolymers which incorporate 2-aceto-1,3-phenanthrenylene units possess higher TgS and increased thermal stability compared to analogous copolymers which have 2-aceto-5-phenyl-1,3-phenylene(biphenyl) or 2-aceto-1,3-phenylene units. Fluorescence spectra of these copolymers have been obtained. 相似文献
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以丙交酯为原料、辛酸亚锡为催化剂、丁二酸酐为改性剂,采用梯度升温法,在150℃、0.098MPa条件下采用直接熔融缩聚法合成端羧基聚乳酸共聚物P(LA/SA),接着用2,2-(1,3-亚苯基)-二 唑啉(1,3-PBO)对其进行扩链,按n(丙交酯)/n(1,3-PBO)= 1/2.4加入1,3-PBO,反应1h制得聚酰胺酯(PEA),最后将高岭土与PEA在150℃、减压条件下熔融复合改性。采用GPC、FTIR、1H NMR、DSC、SEM等手段对聚合物的结构进行表征和性能测试,结果表明,与P(LA/SA) 相比,扩链产物PEA相对分子质量大幅度提高,重均相对分子质量高达24万,玻璃化转变温度Tg高于PLA和P(LA/SA),改性后复合材料的热稳定性能提高,结晶度降低。 相似文献
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Yuan He Xiaohui Wang Hong Zhou Zhiquan Pan Junbo Li Qimao Huang 《Inorganic chemistry communications》2010,13(2):314-318
A new unsymmetrical bis-furan pendant-armed macrocyclic heterodinuclear Cu(II)Zn(II) complex, [CuZnL(OAc)](ClO4)·3MeCN·H2O(1) (H2L was derived from the condensation between 1,6-bis(2-furyl)-2,5-bis(2-hydroxy-3-formyl-5-bromobenzyl)-2, 5-diazahexane and 1,3-diaminopropane), has been synthesized and characterized by EDS (energy dispersive spectroscopy) and X-ray crystallography determination. The interaction between the complex and calf thymus (CT) DNA was investigated by UV–vis absorption, viscosity experiment, fluorescent and CD spectroscopy. The mechanism of the cleavage of supercoiled DNA (pBR 322DNA) process was also studied. It is proposed that DNA cleavage promoted by the complex occurrence via oxidative mechanism. 相似文献
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By using a V-shaped N-containing ligand and a V-shaped carboxylate ligand, we have successfully synthesized a 3D novel copper homochiral coordination polymer, namely [Cu(OPY)(1,3-bdc)]n (complex 1), [1,3-H2bdc = isophthalic acid, OPY = 4,4′-(oxybis(4,1-phenylene))dipyridine]. The compound has been solvothermally synthesized and characterized by IR, elemental analysis, single crystal X-ray diffraction, XRD, UV–vis, and TG analysis. The complex 1 crystallizes in the chiral space group P65 and possesses an unprecedented uninodal 3D 75∙ 8 topology. However, the complex was synthesized by achiral materials. The complex 1 displays a moderate SHG response and its SHG efficiency is about 0.3 times that of urea. In addition, the compound shows high thermal stability. 相似文献
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Five cyclometalated Ir(III) complexes are synthesized from a sulfonate-modified bis-benzimidazole-type organic ligand (3,3′-(2,2′-(1,3-phenylene)bis(1H–benzo [d]imidazole-2,1-diyl))dipropane-1-sulfonic acid, MBS) with different ancillary ligands, and can be classified into two categories. Namely, complexes 1 and 2 (MBS-Ir-ppy and MBS-Ir-Fppy), which are electroneutral, and complexes 3–5 (MBS-Ir-bpy, MBS-Ir-Mebpy, and MBS-Ir-bpyCOOEt), which are cationic and soluble in water. These Ir(III) complexes show tunable luminescence from cyan to orangish red color in solution and yellowish red to pure red color in solid state, with moderately long lifetime (56–528 ns) and high quantum yield (35–71%). 相似文献
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抗菌药伦氨苄西林盐酸盐合成 总被引:4,自引:0,他引:4
以3 羟基丁酮作为起始原料,经过酰氯化、成环、脱氯化氢、溴化合成4 溴甲基 5 甲基 1,3 二氧戊环 2 酮,再和氨苄青霉素反应合成伦氨苄西林盐酸盐。其含量99%,总收率(以3 羟基丁酮计)37.3%。 相似文献