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1.
Moged A. Berghot Nayef S. Almuaikel 《Phosphorus, sulfur, and silicon and the related elements》2013,188(10):1907-1922
Synthesis of 2-anilino-1,4-napthoquinone-3-sulphonyl chloride (2) was achieved from the reaction of the title compound with chlorosulphonic acid. The interesting derivative 2 was used as a building block for synthesis of the sulphonyl derivatives 3–24. All these sulphonyl derivatives were characterized by the physical and spectral data (IR, Mass, 1H- and 13C NMR spectra). 相似文献
2.
Jordanka Petrova Marko Kirilov Snejana Momchilova 《Phosphorus, sulfur, and silicon and the related elements》2013,188(1):29-35
Abstract The reaction of lithium derivatives of N,N,N',N'-tetramethyldiamides of arylmethanephosphonic acids (1-Li) with aldehydes 2 is studied. It is found that under certain reaction conditions (THF, 5 hrs at -70°C and then allowing to warm to room temperature) the aldol stage of the reaction is highly stereoselective, only erythro adducts (2-hydroxyphosphonamides) 3, 4 being formed in 47–75% yields. By heating of 3 and 4 in neutral medium the corresponding (Z)-olefins 5, 6 are obtained (yields 64–74%). It is established that an acid catalyzed olefination of 2-hydroxyphosphonamides is also possible, but the reaction is not stereospecific. 相似文献
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A. Khodairy 《Phosphorus, sulfur, and silicon and the related elements》2013,188(1):159-180
Abstract The reaction of compound 1 with triethyl orthoformate afforded 2, which in turn reacted with CS2 and active methlyene compounds or malononitrile to give dithiolane and 4-malononitrile methylene derivatives 3,4, respectively. Treatment of compound 4 with active methylene compounds afforded spiro cyclopentene derivatives 5a-c. Compound 1 was reacted with bromomalononitrile or CS2 and halocompounds to afford furo-. thieno- and dithiolano-pyrazole derivatives 6–11, respectively. The reaction of compound 12 with phenacyl bromide or benzylidenemalononitrile furnished oxathiol-2-ylidene and pyridinethione derivatives 13,14, respectively. The dibromo derivative 16 was reacted with CS2 and active methylenes or malononitrile to obtain spiro dithietanes 17a-e and 4-dicyano-methlyene derivative 22, respectively. Compounds 17 underwent a cycloaddition reaction with thioglycolic acid, N-phenylbenzohydrazindoyl bromide, 2,5-dimethylfuran and 1-phenyl-3,5-pyrazolidinedi one to give cycloadducts 18–21, respectively. Treatment of > o-aminothiophenol or o-phenylenediamine with the dicyano compound 22 leads to the formation of spiro thiazepine or spiro diazine derivatives 23a,b . The arylidene derivatives 24 was reacted with S,S-acetals, N,S-acetals or ammonium dithiocarbamate to afford dithiane, oxazine or pyrazolodithiocarbamate derivatives 25–29, respectively. Chemoselective cyclization of compound 29 with H2SO4, NaOH or MeI gave compounds 30–32, respectively. Benzopyrano derivatives 34,36 were obtained through the reaction of compound 1 with a mixture of thiourea, triethyl orthoformate and ethyl cyanoacetate or with cyanoketene S,S diacetals, respectively. 相似文献
4.
B. S. Thyagarajan J. A. Simon Nee Glowienka 《Phosphorus, sulfur, and silicon and the related elements》2013,188(1-2):11-18
Abstract A novel synthesis of thiazolidine derivatives is described, based on nucleophilic additions across the triple bond of 1,4-diarylsulfonyl-2-butynes. The use of bidentate nucleophiles like N,N′-dialkylthioureas, under mild base catalysis, at ambient conditions affords good yields of the title compounds. A mechanism for the formation of the compounds is offered and supported by appropriate experiments. 相似文献
5.
Jordanka Petrova Snejana Momchilova Marko Kirilov 《Phosphorus, sulfur, and silicon and the related elements》2013,188(3):243-250
Abstract The reaction of the lithium derivatives of N,N,N′,N′-tetramethyldiamides of arylmethanephosphonic acids (1-Li) with ortho- and para-substituted benzaldehydes 2 is studied. Reaction conditions are found for erythro-stereoselective addition of 1 to 2 with high diastereomeric purity (95–99%) of the erythro adducts 3, 4 (yields 35–72%). By thermolysis of the adducts in neutral medium the corresponding (Z)-ortho and para-substituted stilbenes 5, 6 are obtained. Some factors causing the predominant formation of the erythro adducts 3, 4, as well as the influence of the ortho-substituents on the equilibrium threo-3, 4 ? erythro-3, 4 are discussed. 相似文献
6.
Fawzy A. Attaby Sanaa M. Eldin 《Phosphorus, sulfur, and silicon and the related elements》2013,188(1-4):59-63
Abstract 2-Amino-1.1.3-tricyanoprop-l-ene (1) reacted with thioglycollic acid to afford the key compound for this study namely: 2-amino-I,I-dicyano-3(2-thiazolin-4-on-2-yl)prop-1-ene 2. 2 reacted with hydrazines to afford the thiazolylmethylaminopyrazole derivatives 3 and 4. The reaction of 2 with diazotised primary aromatic amines afforded coupling products which were cyclised to the hydrazothiazolonylpyridazine derivatives 7. The reaction with aromatic aldehydes gave the his-ylidene derivatives 8. Structures are assigned based on elemental and spectroscopic analysis. 相似文献
7.
《合成通讯》2013,43(22):3557-3567
A simple and easy method is provided for the synthesis of the novel pyridinone derivatives (3a–e), (8a–c) and (10a–c) by the reaction of ketene acetals (2a–e), (7a–c) and (9a–c) with ethyl cyanoacetate respectively. Compounds (3b–d) reacted with triethyl orthoformate to afford the pyridinone derivatives (4-6) respectively. Compound 7a reacted with ethyl acetoacetate or diethyl malonate to give thiazolopyridinone derivative 11 or 12 respectively. 相似文献
8.
《Journal of carbohydrate chemistry》2013,32(6):467-483
The xylitol, ribitol and D-arabinitol were transformed into their tributylstannyl ether derivatives by reaction with bis-tributyltin oxide [(nBu3Sn)2O I] and azeotropic removal of water. Subsequent benzyl etherification, using BnBr with solvent or under free solvent conditions, led regioselectively to primary mono-O-benzylalditol derivatives in satisfactory yields for a direct regioselective synthesis (~ 52%). This etherification when applied to tetritols and some hexitols exhibits similar behaviour. With pentitols, an analogous study carried out with the n-dibutyltin oxide [nBu2SnO (II)] as the activating reagent showed contrasting results as regards regioselectivity. 相似文献
9.
Noureddine Raouafi Khaled Boujlel Mohamed Lamine Benkhoud 《Phosphorus, sulfur, and silicon and the related elements》2013,188(12):2471-2482
N-(-1H-Benzimidazol-2-yl) imidates 1a–c react with chlorophosphoramide to give the N-[-1-N,N,N′,N′-tetramethylphosphoramidoyl-1H-benzimidazol-2-yl]-imidates 2a–c or with dichlorophosphoramide to yield the bis[(N-1-benzimidazol-2-yl)-imidate] phosphoramide derivatives 3a–b. The reaction of compounds 2a–c toward primary amines is studied. The obtained amidine derivatives 4a–b were unambiguously characterized by different spectroscopic techniques (IR, 1H, 13C, and 31P NMR, and in some cases MS). 相似文献
10.
Krishna C. Joshi Diwakar Sharma Bidya S. Joshi 《Phosphorus, sulfur, and silicon and the related elements》2013,188(1-4):33-36
Abstract The synthesis of some new sulfur-containing spiroindole derivatives is reported. Fluorinated 3′-aryl-2′-phenylimino-spiro[3H-indole-3,6′[4,5′-pyrazolin][4,3-d]thiazolo]2(1H)-ones were prepared by the reaction of 5-(2-oxo-3-indolinylidene)-3-aryl-2-phenylimino-4-thiazolidinones with hydrazine hydrate. The compounds have been characterized on the basis of elemental and spectral studies. 相似文献
11.
M. A. Metwally E. M. Keshk A. Fekry H. A. Etman 《Phosphorus, sulfur, and silicon and the related elements》2013,188(10):2067-2079
Condensation of thiazolidin-5-one derivative 1 with different aromatic aldehydes gave the corresponding arylidenes 2a–e. Compound 2e was reacted with urea and thiourea to give the corresponding thiazolo[5,4-d]pyrimidine derivatives 3a, b, respectively. Treatment of compound 1 with phenyl isothiocyanate in basic DMF gave the nonisolable potassium salt of the adduct 4, which underwent heterocyclization upon treatment with chloroacetyl chloride and phenacyl bromide to give the corresponding [2,4′] bisthiazolidinylidenes 5 and 8. Moreover, the reactions of compound 1 with a variety of reagents, e.g., ninhydrin and isatin, were investigated. The structures of these compounds were established by analytical and spectral data. 相似文献
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Helmut Duddeck Rainer Lecht 《Phosphorus, sulfur, and silicon and the related elements》2013,188(2-4):169-178
Abstract The syntheses of 16 phenyl- (1 and 3) and phenylthiophosphoryl (2) derivatives are described. The 13C and 17O NMR data sensitively reflect electron density changes in the phosphoryl substituents caused by pπ–dπ back-donation from X/Y to P. Taft constants σ1 and σR 0 were derived for 16 phosphoryl substituents. 相似文献
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《Journal of carbohydrate chemistry》2013,32(7-8):507-517
The synthesis of a number of C-4 and C-9 substituted derivatives of KDN2en methyl ester 2 is reported. 9-Deoxy-9-iodo, 9-azido-9-deoxy and 9-O-methyl derivatives of 2(compounds 5, 7and 9) were prepared from the corresponding 9-O-tosylate, methyl 2,6-anhydro-3-deoxy-9-O-p-toluenesulfonyl-D-glycero-D-galacto-non-2-enonate (3). These compounds have been fully characterised as the peracetates 6, 8 and 10. Treatment of 3 with KSAc gave the 9-thioacetyl derivative which was isolated as the peracetate 11. 4-C-Ethenyl-4-deoxy (14), 4-C-phenyl-4-deoxy (15) and 4-C-[1-(methoxycarbonyl)ethenyl]-4-deoxy (16) derivatives of 2were prepared via the palladium-catalysed coupling of the 4-epi-chloride, methyl 5,7,8,9-tetra-O-acetyl-2,6-anhydro-4-chloro-3,4-dideoxy-D-glycero-D-talo-non-2-enonate (12) with the appropriate organostannanes. 相似文献
16.
Kenneth E. Waters Robert H. Neilson 《Phosphorus, sulfur, and silicon and the related elements》2013,188(3-4):189-197
Abstract The reactions of either PhPCl2 or PCl3 with (Me3Si)2NLi followed by H2C[dbnd]CHMgBr were used to prepare the new P-vinyl substituted [bis(trimethylsilyl)amino]phosphines, (Me3Si)2NP(R)CH[dbnd]CH2 [1: R=Ph, 2: CH[dbnd]CH2, 3: R=Me, and 4: R=N(SiMe3)2]. Oxidative bromination of phosphines 3–1 afforded the P-bromo-P-vinyl-N-(trimethylsilyl)phosphoranimines, Me3SiN[dbnd]P(CH[dbnd]CH2)(R)Br [5: R=Ph, 6: R=CH[dbnd]CH2, 7: R=Me], which, upon treatment with CF3CH2OH/Et3N, were subsequently converted to the P-trifluoroethoxy derivatives, Me3SiN[dbnd]P(CH[dbnd]CH2)(R)OCH2CF3 [8: R=Ph, 9: R=CH[dbnd]CH2, 10: R=Me]. Compounds 1–10, which are of interest as potential precursors to P-vinyl substituted poly(phosphazenes), were fully characterized by elemental analyses (except for the thermally unstable P-Br derivatives 5–7) and NMR spectroscopy (1H, 13C, and 31P) including complete analysis of the vinylic proton splitting patterns via HOM2DJ experiments. 相似文献
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《Journal of carbohydrate chemistry》2013,32(7-8):747-754
A new application of the formazyl activation provided selectively protected new derivatives of both 2-deoxy-D-galactose and 2-acetamido-2-deoxy-D-galactose formazans from 6-amino-6-deoxy-D-galactose 6,4-cyclic carbamate (1) under very simple conditions. The 1H NMR spectrum of the acetylated 2-deoxy derivative 7 revealed an equilibrium between chelated and unusual non-chelated forms of the formazan moiety in solution. 相似文献
20.
Stephan D. Stamatov Stephan A. Ivanov 《Phosphorus, sulfur, and silicon and the related elements》2013,188(3-4):167-171
Abstract A method is proposed for one-pot synthesis of either symmetrical or unsymmetrical diester amidophosphites, developed on the basis of tris-(N,N-dimethyl)-amide/or tris-(N,N-diethyl)-amide/of phosphorous acid, activated by iodine, as a new phosphorylating reagent. Nine thiophosphate, phosphite and phosphite monoester and diester derivatives of 1-O-stearoyl-ethane-2-ol, cholesterol, β-sitosterol and R,S-α-tocopherol have been synthesized under mild conditions (20–75°C) and in high final yields (83--98%). 相似文献