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1.
A new unusual natural pigment from Selaginella sinensis and its noticeable physicochemical properties 总被引:1,自引:0,他引:1
A new unusual pigment with a novel carbon framework named selaginellin (1) was isolated from the acetone extract of Selaginella sinensis, and its methoxy derivative (1a) was synthesized. Both selaginellin 1 and 1a are racemic compounds. The structure of selaginellin 1 was established as (R,S)-4-[(4'-hydroxy-4-(hydroxymethyl)-3-((4-hydroxyphenyl)ethynyl)biphenyl-2-yl)(4-hydroxyphenyl)methylene]-2,5-cyclohexadien-1-one and 1a as (R,S)-4-[(4'-methoxy-4-(methoxymethyl)-3-((4-methoxyphenyl)ethynyl)biphenyl-2-yl)(4-methoxyphenyl)methylene]-2,5-cyclohexadien-1-one by the analysis of one- and two-dimensional NMR data, HR-ESIMS, EI-MS, IR, UV, CD, and single-crystal X-ray experiments, and the mechanism of their color change according to different pH values and fluorescent properties was studied. 相似文献
2.
Wu FY Tan XF Wu YM Zhao YQ 《Spectrochimica acta. Part A, Molecular and biomolecular spectroscopy》2006,65(3-4):925-929
A novel colorimetric sensor based on 8-hydroxy quinoline-5-azo-4'-nitrobenzene (1) was prepared and used for recognizing anions. 1 and its metal complex (1.Co) were found to show response to anions such as CH(3)CO(2)(-), H(2)PO(4)(-), HSO(4)(-), F(-) and dramatic color changes were observed. The selectivity and sensitivity of 1 and 1.Co for sensing anions were different, which was in the order of CH(3)CO(2)(-)>F(-)>H(2)PO(4)(-)>HSO(4)(-) for 1 and H(2)PO(4)(-)>HSO(4)(-)>CH(3)CO(2)(-) approximately F(-) for 1.Co, respectively. In CH(3)CN, sensor 1.Co exhibited excellent specificity toward H(2)PO(4)(-), and the color variety was dependent on the concentration of H(2)PO(4)(-) which was attributed to anion structure and stability of anionic complex (1-anion), metal complex (1-Co) and inorganic complex (Co-anion). 相似文献
3.
Oxidation of the tetraarylpinacols (Ar(2)COH)(2), 1a-e, in which Ar = C(6)H(5) (1a), 4-ClC(6)H(4) (1b), 4-MeC(6)H(4) (1c), 4-MeOC(6)H(4) (1d) and 4-Me(2)NC(6)H(4) (1e), by thianthrene cation radical (Th(*+)) in CH(3)CN and in CH(2)Cl(2) led quantitatively to the corresponding diaryl ketones Ar(2)C=O (2a-e), provided a sufficient amount of base, 2,6-di-tert-butyl-4-methylpyridine (DTBMP), was present to prevent presumed acid-catalyzed rearrangement. In the case of 1e, continued oxidation of 2e was also observed. Oxidation of 1a by (4-BrC(6)H(4))(3)N(*+)SbCl(6)(-) and (4-BrC(6)H(4))(3)N(*+)SbF(6)(-) (Ar(3)N(*+)) occurred analogously. Evidence for the catalytic, cation-radical rearrangement of 1a by Ar(3)N(*+) (reported in earlier literature) and by Th(*+) could not be found. Quantitative oxidation of 1a to 2a and of 1d to 2d was obtained also with NOBF(4), again provided that sufficient DTBMP was present to prevent acid-catalyzed rearrangement. Catalytic, oxidative rearrangement of 1d at room temperature and (as reported in earlier literature) at -5 degrees C was not observed. Oxidation was also observed of 2,3-diphenyl-2,3-butanediol (3) to acetophenone (9) and of 1,1-dimethyl-2,2-diphenylethanediol (4) to 2a and acetone by Th(*+). Oxidation of 2,3-dimethyl-2,3-butanediol (5) by Th(*+) was not observed. Instead, even in the presence of DTBMP, pinacolone (10) and tetramethyloxirane (11) were formed, through, it is proposed, a mechanism involving complexation with Th(*+). 相似文献
4.
合成双酚AF的新方法 总被引:5,自引:1,他引:4
由六氟丙酮三水合物和苯胺,经缩合、重氮化、水解、Friedel-Crafts烷基化等4步反应在常压下合成了双酚 AF。首先,以五氧化二铌为催化剂,在 n (HFA•3H2O) : n (aniline) : n (Nb2O5) = 2 : 1 : 0.1,回流 6 h 条件下,合成出中间体(Ⅰ),收率高达96.3%。然后在重氮化温度为 ﹣2 ~ 2 ℃,硫酸质量分数为 14.7%,n (Ⅰ) : n (H2SO4) : n (NaNO2) = 1 : 4.1 : 1.1,及水解时硫酸质量分数为 50%,n (H2SO4) : n (Ⅰ) = 11.0 : 1、108~112 ℃反应 1.5 ~ 2 h 的优化条件下,化合物Ⅰ经重氮化、水解后以 92.7%的高收率得到中间体 2-(4-羟基苯)六氟异丙醇(Ⅱ);再在甲磺酸存在下,化合物Ⅱ与苯酚经Friedel-Crafts烷基化反应以 72.4% 的收率合成了目标产物双酚 AF(Ⅲ),总收率为 64.6%(以苯胺为基准计算)。 相似文献
5.
R. J. Schiavone C. G. Overberger 《Journal of polymer science. Part A, Polymer chemistry》1988,26(1):107-115
1-Trityl-4-vinylimidazole was prepared by direct tritylation of 4(5)-vinylimidazole and polymerized using a free radical initiator. Poly(1-trityl-4-vinylimidazole) was hydrolyzed using aqueous acetic acid to give poly[4(5)-vinylimidazole]. The poly[4(5)-vinylimidazole], which was obtained from the hydrolysis of poly(1-trityl-4-vinylimidazole), was compared with poly[4(5)-vinylimidazole] prepared directly from 4(5)-vinylimidazole for differences in stereochemistry. The stereochemistry of both polymers was found to be similar by high-resolution NMR. Thus, the trityl does not influence the stereochemistry of poly[4(5)-vinylimidazole]. The reaction of 1-trityl-4-vinylimidazole with n-butyllithium gave 2-lithio-1-trityl-4-vinylimidazole. This intermediate was used to prepare 2-substituted 4(5)-vinylimidazoles, which are new monomers that can be polymerized using free radical initiators. 相似文献
6.
3, 4-Bis (trifluoromethyl)-perfluorohexene-(3) (1) reacted with diethylamine to give the 1-N, N-diethylamino-2-pentafluoroethyl -3-trifluoromethyl-perfluoropentene-(1)(2), which was easily hydrolyzed to the corresponding N, N-diethyl-2-penta-fluoroethyl- 3-trifluoromethyl-perfluoropenteno-(2)-amide (3). When compound 1 was allowed to react with n-butyl amine at 40-50`C, the 2,3,4-tris(trifluoromethyl)-4-pentafluoroethyl-1-n-butyl-aza- cyclobutene-(2) (5) was obtained as the main product and at-30-40`C, 3,4-bis(trifluoromethyl)-4-n-butylamino-perfluorohexene-(2) (4) as the main product. The isomers 3, 4-bis(trifluoromethyl)-4-allyloxy-perfluoro-hexen-(2) (6) and 2-pentafluoroethyl-3-trifluoromethyl-3-allyloxy-perfluoropentene-(1)(7) were formed when 1 was reacted with sodium allyl alcoholate. 相似文献
7.
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
8.
We report a dynamic polymerization system based on the reversible nucleophilic Michael polyaddition of activated alkynes and dithiols. Four poly(dithioacetal)s(P1-P4) were prepared via the base-catalyzed thiol-yne "click" polyaddition of two dithiols(1,4-butanedithiol(4 S) and 1,5-pentanedithiol(5 S)) and two alkynones(3-butyn-2-one(Y1) and 1-phenyl-2-propyn-1-one(Y2)) at high concentrations. We systematically investigated the base-catalyzed polymerization of 4 S and Y1(for polymer P1) under dif... 相似文献
9.
Regioselective alkylation of 2-alkyl-5,6,7,8-tetrahydro-3H-cycloheptimidazol-4-one (1) and 2-alkyl-3H-cycloheptimidazol-4-one (2) was investigated. 3-[2'-(1-tert-Butyl-1H-tetrazol-5-yl)biphenyl-4-ylmethyl]-2-propyl-5,6,7,8-tetrahydro-1H-cycloheptimidazol-4-one (6) was preferentially obtained under the conditions by using NaH in DMF or THF. On the other hand, 3-[2'-(1-tert-butyl-1H-tetrazol-5-yl)biphenyl-4-ylmethyl]-2-propyl-5,6,7,8-tetrahydro-3H-cycloheptimidazol-4-one (5), the synthetic intermediate compound of Pratosartan, was obtained selectively in the presence of n-Bu(4)NBr in toluene by using aqueous sodium hydroxide as a base. In this reaction, it was found that the concentration of the alkaline solution influences its regioselectivity. This selectivity was observed even for aldehyde and ester derivatives. 相似文献
10.
以2,6-二氟苯腈与吗啉反应制得2-氟-6-吗啉-苯腈(1); 1与水合肼在N-甲基吡咯烷酮中通过环合反应制得3-氨基-4-吗啉-1H-吲唑(2); 2与不同羧酸经缩合反应合成了8个新型吲唑类化合物(4a~4h),其结构经1H NMR, IR和HR-ESI-MS表征。抗肿瘤活性测试结果表明:3,4,5-三甲氧基-氮-(4-吗啉-1H-吲唑-3-基)苯甲酰胺(4a)的抗肿瘤活性最好,对K-562, SMMC7721和T-47D肿瘤细胞有明显抑制作用,IC50分别为0.056 μmol·L-1, 0.062 μmol·L-1和0.078 μmol·L-1。 相似文献
11.
Two new glycosides, named Firmacosides A and B, together with known fatty esters, batyl alcohol, Delta(5,20) sterol and sphingosine derivatives have been isolated from the soft coral Sinularia firma TIX-DUR. On the basis of spectroscopic analysis ((1)H-NMR, (13)C-NMR, (1)H-(1)H COSY, HMQC, HMBC and FAB-MS), Firmacoside A was established as hexadecanyl-1-O-alpha-D-arabinopyranosyloxy (1-->4)-alpha-D-arabinopyranosyloxy (1-->4)-alpha-D-arabinopyranoside (1), and firmacoside B was elucidated as docosanyl-1-O-alpha-D-arabinopyranosyloxy (1-->4)-3-O-acetyl-alpha-arabinopyranosyloxy (1-->4)-alpha-D-arabinopyranoside (2). 相似文献
12.
吲哚和2,4-二氯嘧啶经偶联反应制得3-(2-氯嘧啶-4-基)-1H-吲哚(1); 1与CD3I 经取代反应制得3-(2-氯嘧啶-4-基)-1-(甲基-d3)-吲哚(2); 2经两步亲核取代反应制得N′-(2-二甲基氨基乙基)-2-甲氧基-N′-甲基-N-{[4-(1-(甲基-d3)吲哚-3-基)]嘧啶-2-基}-5-硝基苯-1,4-二胺(4); 4经还原反应后,与氯丙酰氯发生缩合反应合成了氘代AZD9291,总收率8.5%,其结构经1H NMR, 13C NMR和ESI-MS表征。 相似文献
13.
N-(Pyren-1-ylmethyl)-(3R,4R)-4-(hydroxymethyl)pyrrolidin-3-ol was synthesised from (3R,4R)-4-(hydroxymethyl)pyrrolidin-3-ol and (3R,4S)-4-[(1S)-1,2-dihydroxyethyl] pyrrolidin-3-ol using alkylation with 1-(chloromethyl)pyrene or reductive amination with pyrene-1-carbaldehyde and NaCNBH3. The incorporation of N-(pyren-1-ylmethyl)azasugar moiety into oligodeoxynucleotides (ODN) as a bulge to form an intercalating nucleic acid (INA) induced a slight destabilization of INA-DNA duplex, whereas the INA-RNA duplex was strongly destabilized and 9 degrees C difference per modification in thermal stability between INA-DNA over INA-RNA duplexes was observed. The stabilization of a DNA three way junction (TWJ) was improved when the intercalator moiety was inserted into the junction region as a bulge. 相似文献
14.
Qiao-Shi Lei Yi-Han Zuo Chang-Zhi Lai Jin-Fang Luo Shu-Wen Pang Hua Zhou Xin-Sheng Yao Jin-Shan Tang 《中国化学快报》2017,28(8):1716-1722
Phytochemical investigations from the roots of Cynanchum stauntonii led to obtain four new C_(21) steroidal glycosides(1–4) and one known compound stauntoside F(5). Their chemical structures were characterized by sophisticated analyses of IR, HRESI-TOF-MS, 1D, and 2D-NMR data, together with chemical methods, which showed interesting 13,14:14,15-disecopregnane-type skeleton or 14,15-secopregnane-type skeleton C_(21) steroidal glycosides. Among them, compound 1 was determined to be glaucogenin C 3-O-b-D-glucopyranosyl-(1 → 4)-b-D-cymaropyranosyl-(1 → 4)-b-D-digitoxopyranosyl-(1 → 4)-b-D-thevetopyranoside. Compound 2 was characterized to be hirundigenin 3-O-a-L-diginopyranosyl-(1 → 4)-b-D-cymaropyranosyl-(1 → 4)-b-D-digitoxopyranosyl-(1 → 4)-b-D-30-demethyl-thevetopyranoside. Compound 3 was identified to be(14S,16 S,20R)-14,16-14,20-15,20-triepoxy-14,15-secopregn-5-en-3-ol-3-O-a-L-cymaropyranosyl-(1 → 4)-b-D-digitoxopyranosyl-(1 → 4)-b-D-oleandropyranoside.Compound 4 was identified to be(14S,16 S,20R)-14,16-14,20-15,20-triepoxy-14,15-secopregn-5-en-3-ol-3-O-a-L-cymaropyranosyl-(1 → 4)-b-D-cymaropyranosyl-(1 → 4)-b-D-digitoxopyranosyl-(1 → 4)-b-Dthevetopyranoside. Among them, compound 2 was hirundigenin type C21 steroidal glycoside that existed in nature as epimers due to the presence of 14-hemiketal hydroxyl group in its structure. In addition, the anti-inflammatory and cardiomyocyte protective effects of compounds 1–4 were evaluated. We found that they exhibited significant protective effects on hypoxia/reoxygenation induced cardiomyocyte injury, but did not showed obvious anti-inflammatory function. 相似文献
15.
Mitsuru Mimura Hiroshi Urakawa Kanji Kajiwara Shinichi Kitamura Kenichi Takeo 《Macromolecular Symposia》1995,99(1):43-55
(1→4)-α- and (1→4)-β-D-linked glucosidic oligosaccharide chains were generated by the Monte Carlo method, and the scattering from the systems composed of simulated chains was calculated to compare with the results of small-angle X-ray scattering from the oligosaccharides in aqueous solution. By extending the simulation to a longer chain, a single chain conformation of (1→4)-α- and (1→4)-β-D-linked polysaccharides was evaluated. On the basis of the simulation, the suprastructure of (1→4)-α- and (1→4)-β-D-linked polysaccharides and their gel formation mechanism were discussed in some detail by analyzing the small-angle X-ray scattering from the aqueous solutions of (1→4)-α- and (1→4)-β-D-linked polysaccharides. 相似文献
16.
枸杞子糖缀合物LbGp4糖链的结构及其免疫活性的研究 总被引:3,自引:0,他引:3
枸杞子糖缀合物LbGp4经β--消除、柱层析分离后得到一条分子量高达180800的分支多糖化合物LbGp4-OL.LbGp4-OL糖基组成为n(Rha):n(Ara):n(Gal)=0.05:1.33:1.根据甲基化、部分酸水解及1HNMR、13CNMR分析,确定了其主要的结构,并对LbGp4和LbGp4-OL的免疫活性进行了研究. 相似文献
17.
微波辐射下2-[4-二-(4-氟苯)甲基]哌嗪乙酰腙化合物的合成 总被引:3,自引:0,他引:3
微波辐射条件下, 以丙酮作溶剂, 1-[二-(4-氟苯)甲基]哌嗪与氯乙酸乙酯反应得到2-[二-(4-氟苯)甲基]哌嗪乙酸乙酯(1), 1与水合肼在微波辐射条件下反应得到2-[二-(4-氟苯)甲基]哌嗪乙酰肼(2), 进一步在微波辐射条件下由2-[二- (4-氟苯)甲基]哌嗪乙酰肼(2)与取代芳香醛反应制得目标化合物3a~3f. 合成的6个目标化合物通过熔点测定和质谱、红外光谱、核磁共振氢谱分析、元素分析对其结构进行确证. 相似文献
18.
Shao Yin ZHANG Xi Gao JIAN* Shu De XIAO Jin Yan WANG Jie ZHANG Department of Polymer Science Materials Dalian University of Technology Dalian 《中国化学快报》2003,14(2)
Poly(aryl ether ketone)s are a category of high performance engineering thermoplastics characterized by high glass transition temperature and excellent thermooxidative stability. And they have important applications in electronic, electric, aircraft and aerospace industries1~3. Considerable efforts have been made towards the improvement of solubility or processability of poly(aryl ether ketone)s4,5. In our work, a novel bis(phthalazinone) monomer 1 4, 4-biphenyl-bis[4-phthalazin-1(2H)-one] … 相似文献
19.
Soluble aromatic polyamides containing phthalazinone moieties were prepared. Those polymers were obtained from the solution polymerization of a new diacid containing phthalazinone moieties with various diamines. The new monomer, 2-(4-carboxyphenyl)-4-(4-carboxyphenoxy)phenyl-1(2H)phthalazinone(Ⅳ) was synthesized in a two-step reaction sequence. 2-(4-Cyanophenyl)-4-(4-cyanophenoxy)phenyl-1(2H)phthalazinone (Ⅲ) was prepared via the condensation reaction of 4-(4-hydroxyphenyl)-1(2H)phthalazinone (Ⅰ) with p-chlorobenzonitrile (Ⅱ). After (Ⅲ) was hydrolyzed, (Ⅳ) was acquired. The synthesized polyamides were characterized by means of viscosimetry, DSC, FT-IR, 1H NMR and EA. The polyamides have a high glass transition temperature which can be as high as 316 ℃. The polyamides also have good solubilities in some organic solvents. 相似文献
20.
在碘化亚铜、四丁基溴化铵和磷酸钾存在下,9,9-二(4-羟基苯基)呫吨(1)和4-甲基碘苯(2)于N,N-二甲基甲酰胺溶剂中发生Ullmann偶联反应,加热回流反应24 h,以95%的产率合成了中间体--9,9-二[4-(4-甲基苯氧基)苯基]呫吨(3),继而加入催化量的N-溴代丁二酰亚胺并在光照条件下,将中间体3氧化得到一种新型芳香族二羧酸--9,9-二[4-(4-羧基苯氧基)苯基]呫吨(4),其产率为84%,二步反应总收率为79.8%。 目标化合物4经1H NMR、13C NMR、IR和元素分析测试技术确定了其结构。 该法具有原料易得,操作简单,反应条件温和,收率高等优点。 相似文献