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1.
Witold Przychodzeń 《Phosphorus, sulfur, and silicon and the related elements》2013,188(8):1621-1633
Reaction of the Lawesson's reagent (LR) with aliphatic 1,2- and 1,3-diols as well as with aromatic 2,2′-dihydroxybiphenyl led to new products. Stable di-tert-butylammonium salts of bis-anisyldithiophosphonic acids 6 were isolated and were then converted into unique 9-, 9-, and 10-membered cyclic disulfides 7 and into S,S-dimethyl esters 8. The salts of bis-anisyldithiophosphonic acids 6 were shown to be capable of splitting the disulfide bond of Ellman's reagent. 相似文献
2.
Il'yas S. Nizamov Alexey E. Popovich Elvira S. Batyeva Nail M. Azancheev Vladimir A. Al'fonsov 《Phosphorus, sulfur, and silicon and the related elements》2013,188(1):167-178
Abstract The reactions of tetraphosphorus decasulfide and Lawesson's reagent with tetra-, tri- and dialkoxysilanes were studied. On the basis of these reactions, new S-silyl esters of phosphorus(V) thioacids have been prepared. The prepared compounds were identified by IR, 1H, and 31P NMR and mass spectra as well as elemental analyses. 相似文献
3.
Erdal Ertas Hakan Bildirir Onur Sahin Ipek Oksen 《Phosphorus, sulfur, and silicon and the related elements》2013,188(12):1835-1844
Abstract Syntheses of two analogues of tetrathiafulvalene (TTF), fused to 1,4-dithiin and thiophene rings, substituted with thiophene moieties, have been illustrated. The syntheses were accomplished through the reaction of a 1,8-diketone with phosphorus pentasulfide or Lawesson's reagent in boiling dry toluene. Conversion of the thioketones to their the oxo forms with mercury (II) acetate, was followed by self-coupling in freshly distilled boiling triethyl phosphite. Attempts for their electro-polymerizations through the thiophene groups at the peripherals were unsuccessful. Computational chemistry studies revealed that the thiophene groups did not exhibit enough spin densities to perform polymerization. Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file. 相似文献
4.
P. Manivel S. Mohana Roopan D. Prem Kumar F. Nawaz Khan 《Phosphorus, sulfur, and silicon and the related elements》2013,188(10):2576-2582
A series of 3-substituted-1H-isochromene-1-thiones (3) were prepared by the reaction of 3-substituted isocoumarins (2) with Lawesson's reagent in the presence of toluene under a nitrogen atmosphere. The antimicrobial activities of the newly synthesized products were measured using Gram-negative (Escherichia coli, Salmonella typhi, and Proteus mirabilis) and Gram-positive bacteria (Staphylococcus aureus and Bacillus cereus). Synthesized thioanalogue of isocoumarins showed good antibacterial activity against Proteus mirabilis. 相似文献
5.
Abd El-Badih A. G. Ghattas Hassan M. Moustafa Elsayed A. A. Hassanein Bahgat R. M. Hussein 《Phosphorus, sulfur, and silicon and the related elements》2013,188(12):1469-1481
Abstract Alkylation of 4-anilino-5-phenyl-4H-1,2,4-triazole-3-thiol (1) with some halo compounds yielded the corresponding sulfides 2a–f. Some sulfides 2e,f were cyclized to give triazolothiadiazines 3 and 4. Triazolothiadiazoles 5 and 6 were prepared through the reaction of compound 1 with carbon disulfide or ethyl orthoformate, respectively. Treatment of compound 1 with ethyl chloroformate or phenyl isothiocyanate yielded triazolo-thiadiazole and triazole 9 and 10, respectively. Reaction of compound 1 with Lawesson's reagent gave triazolothiadiazaphosphole derivative 11. Also, compound 1 underwent cyclocondensation reactions with some bidentate reagents to give triazolothiazines 4, 12, and 13. Triazolo-thiazepines and triaziepine 14–16 were synthesized via the reaction of compound 1 with β-ketoesters or ethyl cyanoacetate. Tricyclic systems 19 and 20 were prepared through the reaction of compound 4 with the appropriate reagent. Some synthesized compounds were tested for antibacterial activity. Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file. 相似文献
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Soher S. Maigali Fouad M. Soliman Rashad Shabana Marwa El-Hussieny 《Phosphorus, sulfur, and silicon and the related elements》2013,188(9):2408-2426
The reaction of Lawesson's reagent 1a, with niclosamide 2 proceeded by thionation and formation of carbothioamide 3 and the zwitterionic oxathiaphosphinin 4a. LR reacted with 8-hydroxyquinoline (5), 2-methylquinoline-4-ol (7), and β-naphthol (9) to give the phosphonodithioates 6, 8, or 10. The reaction of LR with the Mannich bases 11 and 14 afforded the oxathiaphosphinins 13 and 15, whereas the phosphonodithioates 17 and 19 were isolated in the case of Mannich bases 16 and 18. LR reacted with phthalimide Mannich base 20 to give the dithione 21 and N-methylphthalimide (22). Reaction of ketone monoxime 23 with LR resulted in the formation of the oxathiaphosphole 24 and the dithiaphosphole 25, whereas the monoxime 26 afforded the thioxoethanone thioxime 27. Ketone dioximes 28 and 34 afforded the phosphonodithioates 29 and 36, respectively, when they were allowed to react with LR, whereas the dioxime 30 gave compounds 32 and 33. Moreover, the molluscicidal potency of the newly synthesized compounds against Biomphalaria glabrata snails was studied, too. 相似文献
8.
One‐Pot Approach to Organo‐Phosphorus–Chalcogen Macrocycles Incorporating Double OP(S)SCn or OP(Se)SeCn Scaffolds: A Synthetic and Structural Study
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Dr. Guoxiong Hua Junyi Du Prof. Alexandra M. Z. Slawin Prof. J. Derek Woollins 《Chemistry (Weinheim an der Bergstrasse, Germany)》2016,22(23):7782-7791
The development of new methodology for the preparation of functional macrocycles with practical applications is an important research area in macromolecular science. In this study, we report a new one‐pot route for the synthesis of a series of macro‐heterocycles by incorporating two phosphorus atoms and two chalcogen atoms and two oxygen atoms (double OP(S)SCn or OP(Se)SeCn scaffolds). The three‐component condensation reactions of 2,4‐diferrocenyl‐1,3,2,4‐diathiadiphosphetane 2,4‐disulfide ( FcLR , a ferrocene analogue of Lawesson's reagent) or 2,4‐bis(4‐methoxyphenyl)‐1,3,2,4‐dithiadiphosphetane 2,4‐disulfide ( LR , Lawesson's reagent), or 2,4‐diphenyl‐1,3,2,4‐diselenadiphosphetane 2,4‐diselenide ( WR , Woollins’ reagent), disodium alkenyl‐diols, and dihalogenated alkanes are performed, giving rise to soluble and air or moisture‐stable macrocycles in good‐to‐excellent yields (up to 92 %). This is the first systemically preparative and readily scalable example of one‐pot ring opening/ring extending reaction of three‐components to prepare phosphorus–chalcogen containing macrocycles. We also provide a systematic crystallographic study. 相似文献
9.
Unsubstituted and substituted linear polythienyls including thiophenes in both even and odd numbers are conveniently prepared from the Michael addition of thiophenecarboxaldehydes to Mannich bases and the vinyl sulfone. Cyclization of the resulting 1,4-diones with Lawesson's reagent gives α-polythienyls. 相似文献
10.
Synthesis of new benzoxazaphosphinine/benzoxazaphosphole/diazaphosphaphenalene 2‐sulfides were accomplished by the reaction of Lawesson's reagent (LR) with 4‐bromo‐2‐[(phenylamino) methyl]phenol (1a), 4‐bromo‐2‐[(4‐chloro/bromo/methoxy/methylphenyl‐amino)methyl]phenol (1b–e), 4‐bromo‐2‐[(benzylamino)methyl]phenol (1f), 2‐amino‐4‐chlorophenol (2a)/2‐amino‐4‐methylphenol (2b), 1,8‐diaminonaphthalene (3) respectively in anhydrous toluene. Products 4a–f, 5a–b and 6 were characterized by IR, 1H, 13C, 31P NMR and Mass spectra. 相似文献
11.
Maaroof Zarei 《Tetrahedron》2017,73(14):1867-1872
A simple and efficient synthetic method for the one-pot synthesis of 1,3,4-thiadiazoles utilizing Vilsmeier reagent was developed. In this method carboxylic acids and hydrazine were converted to 1,3,4-thiadiazoles in the presence of Vilsmeier reagent and Lawesson's reagent. The influence of the thionation reagent, solvent, temperature and time, in this reaction was discussed. The developed methodology for 1,3,4-thiadiazole synthesis has the advantage of simplicity, ambient reaction conditions, easy purification and good to excellent yield of products. 相似文献
12.
Fayaz Ali Larik Aamer Saeed Urooj Muqadar Hesham El-Seedi Muhammad Faisal Pervaiz Ali Channar 《Phosphorus, sulfur, and silicon and the related elements》2017,192(5):490-502
This review, including 111 references, describes the applications of Lawesson's reagent (LR) [2,4-bis(p-methoxyphenyl)-1,3,2,4-dithiadiphosphetane-2,4-dithione] for the total synthesis of macrocyclic natural products. LR is a versatile reagent and shows excellent regioselectivity, chemoselectivity, and offers the products in high yield. The thionation of carbonyl moieties present in macrocyclic natural products, and cyclization to construct key heterocyclic fragments is described. Moreover, this review highlights the medicinal significance of the natural products. 相似文献
13.
Ethyleneglycol derivatives of 2-methyl (and ethyl)-3-hydroxy-4-pyridinone were synthesized by a modified Hilbert-Johnson reaction. The synthesis proceedes by reaction of O-protected 2-alkyl-3-hydroxy-4-pyridinone with hexamethyldisilazane in the presence of chlorotrimethylsilane followed by trimethylsilyl trifluoromethanesulfonate catalized alkylation with benzyloxy-ethoxymethylchloride in dichloroethane and deprotection by hydrogenation. The overall yield was 87%. This method provides a useful way to produce oligo- or polyethyleneglycol substituted hydroxypyridinones. 相似文献
14.
Liangnian He Yanping Luo Kai Li Guangfu Yang Mingwu Ding Xiaopeng Liu 《Phosphorus, sulfur, and silicon and the related elements》2013,188(11):2675-2678
A convenient one-pot synthesis of fused phosphorus-heterocycles with biological activity via the cyclization reactions of Lawesson's reagent with bifunctional substrates is reported. 相似文献
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Ertuğrul Gazi Sağlam Ömer Çelik Hamza Yılmaz Nurcan Acar 《Phosphorus, sulfur, and silicon and the related elements》2013,188(11):1339-1346
Abstract Potassium and tetraphenylphosphonium salts of novel aryldithiofluorophosphonic acids were synthesized. Lawesson's Reagent was allowed to react with KF in acetonitrile to yield the potassium salt of p-methoxyphenyldithiofluorophosphonic acid. Treatment of the latter with tetraphenylphosphonium chloride resulted in the formation of the tetraphenylphosphonium salt. The structures of the compounds were elucidated by FTIR, 1H, 13C, 19F, and 31P NMR spectroscopy as well as by ESI-mass spectrometry. The molecular and crystal structure of the tetraphenylphosphonium salt, determined by single crystal X-ray diffraction, is also presented. Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file. 相似文献
17.
茉莉酮和二氢茉莉酮是一类名贵的香料,此类化合物的合成一直是人们所关注的问题。已有许多报道,其中包括庚醛、1-硝基庚烷与甲基乙烯基酮进行Michael加成和以硝代甘缩酮与庚醛进行硝-醛缩合制得1,4-二酮,再进行分子内缩合为二氢茉莉酮。这些合成方法,有的对反应条件要求较苛刻,不易操作,有的则反应步骤较多,收率低。最近,白俊才等以甲基乙烯基酮和1-己烯为原料,合成了二氢茉莉酮,此法虽然新颖,但氧硼杂环己烷中间体 相似文献
18.
S. S. Krishnamurthy K. Ramachandran A. C. Sau M. N. Sudheendra Rao A. R. Vasudeva Murthy R. Keat 《Phosphorus, sulfur, and silicon and the related elements》2013,188(1):117-119
Abstract The 31P nmr spectra of 2,4- and 2,6-diamino-derivatives of octachlorocyclotetraphosphazatetraene, N4P4Cl6(NR1R2)2 (R1 = H, R2 = But; R1 = H, R2 = CH2Ph; R1 = Me, R2 = Ph), have been measured. The 2,4- and 2,6-isomers were analysed as AA'BB' and A2B2 spin systems respectively. In the 2,4-isomers the spin-spin couplings 2J(PNP) and 4J(PNPNP) were of opposite sign. 相似文献
19.
A. Khodairy H. Abdel-ghany 《Phosphorus, sulfur, and silicon and the related elements》2013,188(1):259-273
Abstract 3,4-Diamino-2,5-dicarbethoxythieno(2.3-b)thiophene 1 reacted with malononitrile or ethyl cyanoacetate to afford bis(thienopyrimidin-4-one) derivatives 2a.b The reaction of compound 1 with o-aminothiophenol, o-aminophenol or o-phenylenediamine gave benzothiazolyl-, benzoxazolyl-, benzoimidazolylthienothiophene 3a-c, Chloroacetylation of compound 1 and reacting the resulting compound 4 with malononitrile furnished thienopyrolopyrimidine 6. Fusion of compound 1 with formamide yielded bis(thienopyrimidine) 7 which reacted with POCI3/PCl5 to yield the corresponding chloro derivative 8 which was converted into the corresponding hydrazine derivative 9. Treatment of compound 1 with CS2, NaOH and 1,2 dibromoethane produced the corresponding 1.3 dithiolane 11 which also treated with chloroacetyl chloride or ethyl mercaptoacetate to get the corresponding β-lactame 12 or thiazolidinone 13. On reacting compound 1 with CS2, NaOH and (CH3)2S04 produced the corresponding bi(dithiocarbamate methyl ester) 14 which treated with hydrazine hydrate to yield the corresponding bis(thienopyrimidine) derivative 15. This compound reacted with Lawesson's reagent (LR) to give the desired compounds 16 and 17. While its reaction with (CH3)2 SO4 and NaOH furnished the corresponding methyl derivative 18. Fusion of compound 18 with aniline afforded compound 19. Compound 19 was allowed to react with ethyl acetoacetate, acetylacetone, α-oxoketene dithioacetal, ethoxymethylene malononitrile or LR to get the described compounds 2Oa.b-24 respectively. 相似文献
20.
聚对苯乙炔 (PPV)及其衍生物是制备聚合物发光二极管的最重要的聚合物之一[1] .这主要是因为它们具有优越的电致发光性能 ,易于合成以及良好的环境稳定性[2 ] .而聚 (2 甲氧基 5 (2′ 乙基 己氧基 ) 对苯乙炔 ) (MEH PPV)由于其可溶性好 ,发光效率和亮度高 ,在电致发光领域广受关注 .现在有许多MEH PPV的多步化学合成方法以及电化学合成方法 .但是 ,这些方法常常产率低 ,成本高且产品不纯 .本文报道一种固 液两相反应一步合成分子量大、溶解性好的MEH PPV的新方法 .1 主要原料对甲氧基苯酚 (纯度≥ 98% ,Aldr… 相似文献