Über Das Kernresonanzspektrum Der Vinylgruppe

Brügel, Werner; Ankel, Th.; Krückeberg, F.

doi:10.1016/b978-1-4832-1330-9.50047-9

Cited by 10 publications

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“…Although the spectra for some of these compounds have been reported previously by other workers (3)(4)(5)(6)(7)(8) 46,1968 Happe (6) are roughly 40% higher and 20% lower respectively than the corresponding coupling constants reported by Briigel and co-workers (3). Considerable difficulties have .…”

Section: Introductionmentioning

confidence: 52%

“…A striking example of such a system is the spectrum of SiVi,. Despite a number of attempts (3)(4)(5) to determine a correct set of parameters by iterative and exact methods (4) at two different frequencies (40 and 60 MHz) the parameters were still in question until accurate values of the coupling constants were obtained from the I3C satellite spectra (5).…”

Section: Discussionmentioning

confidence: 99%

“…Considerable difficulties have . , also been encountered in obtaining an unambiguous analysis of the SiVi, spectrum (3)(4)(5). The problem in the latter case has been largely resolved by determining the proton couplings from the I3C satellite spectra (5).…”

Section: Introductionmentioning

confidence: 99%

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Proton magnetic resonance spectra of vinylmetallic compounds. Part I. Tetravinyl and triphenylvinyl derivatives of Group IVB elements

Cawley¹,

Danyluk²

1968

Can. J. Chem.

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A study has been made of the proton magnetic resonance spectra for all of the Group IVB derivatives of the series MVi, and 43MVi (4 = phenyl group and Vi = vinyl group). The spectra were measured at 60 MHz as accurately as possible and the assignment of transitions was checked with a variety of supplemental aids including double irradiation, nlultiple quantum transitions, and medium effects. Final, accurate spectral parameters were derived using both iterative and exact comp~~tational methods for solution of the three-spin problem. Excellent agreement was obtained between the sets of parameters determined by the two methods.The clien~ical shifts for both series of compounds display a nunlber of characteristic trends of which the most notable is a displacenlent of the vinyl proton signals to low field with increasing atomic number of the M atom. In each series the largest shift change is noted in going from the carbon to the silicon dcrivative. These deshicldings have been attributed to the enhanced possibility of d,-p, interaction between the central M atoll1 and the vinyl group in higher nlenlbers of the series. Marked changes are also noted for the internal shifts of the vinyl protons down both series of compounds. It is concluded that these changes are principally due to the effects of the M-C bond diamagnetic anisotropy. The trends in internal shifts can be satisfactorily reproduced by the dipole approxin~ation using AX values of 4, 6, 8, 12, and 18 x cnl3 mole-' for the C, Si, Ge, Sn, and Pb-carbon bonds respectively. The signals for the vinyl protons of the &MVi series are all located to low field relative to the MVi, series. This deshielding is satisfactorily accounted for by the effects of the phenyl ring diamagnetic anisotropy in the former series.A linear correlation is observed between the sums of the coupling constants and the electronegativities, Em, of the central M atom for both series of compounds. However, the XJvalues for the &MVi series are all slightly lower than the corresponding s u n~s for the MVi4 series, indicating that the electronegativity of the phenyl group is somewhat larger than for the vinyl group.A significant solvent and concentration dependence is only noted for compounds belonging to the &MVi series. For examplc, the tratis proton of +3GeVi shifts up-field by 4 Hz while the cis proton is displaced down-field by 4 Hz as the concentration of 4,GeVi is increased to 50 mole % in carbon tetrachloride. These changes have been interpreted on the basis of a solute-solute interaction scheme of the type proposed previously for phenyl proton shifts.

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Section: Introductionmentioning

confidence: 52%

Section: Discussionmentioning

confidence: 99%

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Proton magnetic resonance spectra of vinylmetallic compounds. Part I. Tetravinyl and triphenylvinyl derivatives of Group IVB elements

Cawley¹,

Danyluk²

1968

Can. J. Chem.

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“…spectrum ofisoquinoline (12,13) only a few spectra of substituted isoquinolines have been studied (14)(15)(16).…”

Section: Nuclear Magnetic Resonance Spectramentioning

confidence: 99%

“…5-Amino-8-mercaptoiroqirinoline (14) A solution of 2.0 g (0.01 mol) of 5-amino-8-thiocyanoisoquinoline (13) in 120 ml of 8 N hydrochloric acid and 120 ml of ethanol was refluxed for 4 h. -1 he acid solution was evaporated to dryness on a water bath leaving a yellow solid, which was dissolved in 50 ml of water. Neutralization of the solution with sodium carbonate solution produced a precipitate which was filtered and Can.…”

Section: 5-diacetamidofhiazololr54-h]isoquinolinementioning

confidence: 99%

Thiazoloisoquinolines. IV. The Synthesis and Spectra of Thiazolo[4,5-h]- and Thiazolo[5,4-f]isoquinolines. The Ultraviolet and Proton Magnetic Resonance Spectra of Some Substituted Isoquinolines

Taurins¹,

Hsia²

1971

Can. J. Chem.

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Thiazolo[4,5-hlisoquinoline was synthesized from 7-aminoisoquinoline in four steps: by the reaction with potassium thiocyanate and bromine to give 7-amino-8-thiocyanoisoquinoline; cyclization of the latter with hydrochloric acid to produce 2-aminothiazolo[4,5-h]isoquinoline, followed by the Sandmeyer reaction to yield a 2-chloro derivative, and finally, reduction with hydriodic acid and phosphorus.Thiazolo[5,4-f]isoquinoline was prepared from 6-aminoisoquinoline via 6-amino-5-thiocyanoisoquinoline. The synthesis of 2,5-diaminothiazolo [5,4-hlisoquinoline was achieved by cyclization of 5-acetamido-8-aminoisoquinoline which was obtained from 5-aminoisoquinoline. In 5-amino-8-thiocyano-and 8-amino-5-thiocyanoisoquinolines, the thiocyano group was hydrolyzed to the thiol group with 8 N hydrochloric acid and ethanol (1 :l).The U.V. and p.m.r. spectra of the intermediate isoquinolines, and the i.r., u.v., and n.m.r. spectra of thiazoloisoquinolines were studied.On a synthetist le thiazolo[4,5-h]isoquinoline a partir de la 7-aminoisoquinoline en quatre Btapes: par la reaction avec le thiocyanate de potassium et le brome, on obtient le 7-amino-8-thiocyanoisoquinoline; la cyclisation de ce produit avec I'acide chlorhydrique amene au 2-aminothiazolo [4,5-hlisoquinoline, suivi par la reaction de Sandmeyer, ce qui donne le derive 2-chloro dont on fait la reduction avec l'acide iodhydrique et le phosphore. On a prepart le thiazolo[5,4-flisoquinoline a partir du 6-aminoisoquinoline en passant par le 6-amino-5-thiocyanoisoquinoline. On a reussi la synthese du 2,5-diaminothiazolo- [5,4-h]isoquinoline qui fut obtenu a partir du 5-aminoisoquinoline. Pour les 5-amino-8-thiocyano-et le 8-amino-5-thiocyanoisoquinolines, le groupe thiocyano a ete hydrolyse en thiol avec l'acide chlorhydrique 8 N e t l'Bthanol(1 :1).On a etudie les spectres ultraviolet et de r.m.p. des isoquinolines intermidiaires, de m6me que les spectres i.r., u.v., et r.m.n. des thiazoloisoquinolines.

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Formierung einer wissenschaftlich-technischen Gemeinschaft

Reinhardt

Steinhauser

2008

N.T.M.

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The Formation of a Scientific-technological Community. NMR-Spectroscopy in the Federal Republic of Germany After World War II, different kinds of physical instruments became the cores of communities whose members were specialised in the development of instrumental methods. Scientists, instrument builders, civil servants, and employees of private companies took over active parts in the formation of these communities. In his concept of Research Technology, the sociologist Terry Shinn identified a specific group between scientific research and technology of instrumentation, working on the invention of instruments and their transfer into different fields of application. Here, we focus on the final part of this process. Our case study is the implementation of Nuclear Magnetic Resonance (NMR) in the Federal Republic of Germany as a standard method for spectroscopical analysis in chemistry, and as a research field in its own right. In this setting, the adaptation and institutional stabilisation of NMR in chemistry cannot be reduced to the activities of the relatively narrow group of research technologists. We call the social network around NMR a scientific-technological community. Like research technologists, members of the scientific-technological community worked in the interstitial spaces between science, administration, and industry, but they comprised a much wider range of functions. As for results, we recognize the huge impact of governmental funding on the innovation of novel instrumentation, the importance of academic scientists as both referees and users, and the efforts to establish NMR as a truely interdisciplinary field and generic method. The case of NMR in the Federal Republic of Germany shows specific regional traits, but is part of a general movement in science emphasizing the development of instrumental methods.

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Über Das Kernresonanzspektrum Der Vinylgruppe

Cited by 10 publications

References 0 publications

Proton magnetic resonance spectra of vinylmetallic compounds. Part I. Tetravinyl and triphenylvinyl derivatives of Group IVB elements

Proton magnetic resonance spectra of vinylmetallic compounds. Part I. Tetravinyl and triphenylvinyl derivatives of Group IVB elements

Thiazoloisoquinolines. IV. The Synthesis and Spectra of Thiazolo[4,5-h]- and Thiazolo[5,4-f]isoquinolines. The Ultraviolet and Proton Magnetic Resonance Spectra of Some Substituted Isoquinolines

Formierung einer wissenschaftlich-technischen Gemeinschaft

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