| 81 | Author
| Ulrich Knips, Friedo Huber | Requires cookie* | | Title
| Umsetzungen von Monomethylthalliumdiacetat mit Aminen Reactions of Monomethylthallium Diacetate and Amines  | | | Abstract
| Decomposition of MeTl(OAc)2 (Me = CH3, HO Ac = CH3COOH) in methanol in the presence of amines, like 2-, 3-and 4-picoline, benzylamines, dimethylaniline causes mainly N-methylation; the concurring O-methylation of acetate, giving MeOAc, is only of minor importance. The rate of N-methylation increases in the series 2-picoline < pyridine < 3-picoline < 4-picoline < dimethylaniline < dime thy lbenzylamine. Picolinic acid and MeTl(OAc)2 (molar ratio 1:1) react to give 25% N-methylpicolinic acid and 75% MeOAc; when the molar ratio was at least 2:1, a 1:1 mixture of N-methylpicolinic acid and the methylester of picolinic acid was produced. These results and rate changes in different solvents are explained by assuming MeT10Ac+ being the active methylthallium electro-phile. Der geschwindigkeitsbestimmende Schritt beim Zerfall von Monomethylthalliumverbindungen MeTlX2 (Me = CH3, X = z.B. CH3COO) in Lösung kann als S^-Angriff des jeweils stärksten Nukleo-phils oder konkurrierender Nukleophile (Anion und Solvensmoleküle) im Reaktionssystem an der Tl-gebundenen Methylgruppe von MeTlX+ verstanden werden, das im Dissoziationsgleichgewicht mit MeTlX2 vorliegt [1,2]. Weitere Untersuchungen der Zerfallsreaktion in Gegenwart organischer Amine, über die wir nachfolgend berichten, bekräftigen diese Vorstellung und erlauben Aussagen über den Einfluß von Nukleophilie und Basizität der Reak-tanden bei diesen Zersetzungsreaktionen. Ergebnisse Beim Zerfall von MeTl(OAc)2 in methanolischer Lösung in Gegenwart von 2-, 3-und 4-Picolin ent-standen in allen Fällen als Hauptprodukte die ent-sprechendenN-Methylpicoliniumacetate und T10 Ac. Daneben bildete sich Essigsäuremethylester (MeOAc) in einer von der verwendeten Base ab-hängigen Menge: So wurden bei Verfolgung des Zerfalls von MeTl(OAc)2 in Gegenwart von 2-bzw. 3-bzw. 4-Picolin nach 20 h bei einer Reaktions-temperatur von 30 °C etwa 15 bzw. 5 bzw. 2-3% MeOAc (bezogen auf die berechnete maximale Menge von MeOAc als einziges Zerfallsprodukt) gefunden. | | |
Reference
| Z. Naturforsch. 38b, 434—436 (1983); eingegangen am 20. Dezember 1982 | | |
Published
| 1983 | | |
Keywords
| Monomethylthallium Diacetate, Amines, Methylation, Reaction Rate | | |
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| default:Reihe_B/38/ZNB-1983-38b-0434.pdf | | | Identifier
| ZNB-1983-38b-0434 | | | Volume
| 38 | |
82 | Author
| Hans Dörner, Kurt Dehnicke, Werner Massa, Roland Schmidt | Requires cookie* | | Title
| Synthesis, IR Spectrum and Crystal Structure of a,a'-Dipyridyldi(iodineazide)  | | | Abstract
| Preparation, a,a'-Dipyridyldi(iodineazide), IR Spectrum, Crystal Structure The complex [a,a'-dipyridyl(IN3)2] can be prepared by reaction of a,a'-dipyridyl with iodine azide in CH2CI2 solution. It forms stable, yellow, moisture-sensitive crystals of melting point 73 °C. According to the IR spectrum the IN3 molecules are covalently bonded to the N atoms of the dipyridyl via the iodine atoms. The crystal structure deter-mination was carried out by X-ray methods (2127 independent reflexions, R = 3.2%). The complex crystallizes in the space group P2i/c with four formula units per unit cell, (a = 1299, b = 726, c -1647 pm; ß = 96.1°). The IN3 molecules form linear bridges Na-I-N to the nitrogen atoms of the pyridyl rings with bond lengths Na-I 217 pm and Npyr-I 244 pm. The dihedral angle of the pyridyl rings is 63.4°. | | |
Reference
| Z. Naturforsch. 38b, 437—441 (1983); eingegangen am 10. Dezember 1982 | | |
Published
| 1983 | | |
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| default:Reihe_B/38/ZNB-1983-38b-0437.pdf | | | Identifier
| ZNB-1983-38b-0437 | | | Volume
| 38 | |
84 | Author
| Martin Hoch, Dieter Rehder | Requires cookie* | | Title
| Carbonylniobium Chemistry, IV [1] Derivatives of ^ 5 -C5H5Nb(CO)4 with Tridentate Phosphines  | | | Abstract
| The photo-induced reaction between CpNb(CO)4 and Ph2P(CH2)2PR(CH2)2PPh2 (L; R = Ph, Cy) yields the chelated five-membered ring complexes cis-[CpNb(CO)2L] (two isomers in the case of R = Cy). The uncordinated PPI12 group reacts with CpNb(CO)3THF to form CpNb(CO)2(ia-L)CpNb(CO)3. IR, 31 P and 93 Nb NMR spectra are discussed and compared with corresponding data of the analogous vanadium complexes. | | |
Reference
| Z. Naturforsch. 38b, 446—448 (1983); received December 17 1982 | | |
Published
| 1983 | | |
Keywords
| Carbonylniobium, 1, 4, 7-Triphosphaheptanes, 31 P NMR, 93 Nb NMR | | |
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| default:Reihe_B/38/ZNB-1983-38b-0446.pdf | | | Identifier
| ZNB-1983-38b-0446 | | | Volume
| 38 | |
85 | Author
| PeterG. Jones, GeorgeM. Sheldrick, Rafael Usón, Juan Forniés, MiguelA. Usón | Requires cookie* | | Title
| Dithiocarbonate and Trithiocarbonate Complexes of Palladium(II); Crystal Structure of Pd(Ph3P)2(CS20) CH2C12  | | | Abstract
| Dithiocarbonate, Trithiocarbonate, Palladium(II), Crystal Structure Di-and trithiocarbonate complexes of palladium(II) have been prepared by the action of 02 or Ss on PdL2(?7 2 -CS2) in the presence of excess L (L = phosphine ligand). 31 P NMR data for Pd(PPh3)2(CS20) are consistent with the presence in solution of both S,S and S,Q coordinated dithiocarbonate. An X-ray crystal structure of the dichloromethane solvate [PI, a = 1103.6(4), b = 1343.4(5), c = 1368.5(5) pm, a = 94.77(3), ß = 94.67(3), y = 113.64(3)°, Z = 2, R — 0.059] suggests that an equivalent disorder may occur in the solid state. | | |
Reference
| Z. Naturforsch. 38b, 449—453 (1983); received November 2 1982 | | |
Published
| 1983 | | |
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| default:Reihe_B/38/ZNB-1983-38b-0449.pdf | | | Identifier
| ZNB-1983-38b-0449 | | | Volume
| 38 | |
86 | Author
| Hans-Ulrich Höfs, Rüdiger Mews, Mathias Noltemeyer, GeorgeM. Sheldrick, Martin Schmidt, Gerald Henkel, Bernt Krebs | Requires cookie* | | Title
| Reactions of Fluorinated Nitriles with Sulphur(II) Chlorides; Crystal Structure of 2,4,6-Tris(difluorosulphoximido)-l,3,5-triazene at 170 K  | | | Abstract
| The addition of CF3SC1 (2) to the fluorinated nitriles RfCN[Rf = CF3 (3), NSF2 (4), NSOF2 (5)] leads to N-perfluoromethanesulphenyl-formylimidoylchlorides CF3S-N = C(C1)/?/ (6, 11, 12). From the reactions of SC12 (1) with (3) and (5), which yielded the N-sulphenyl-chlorides C1S-N = C(C1)-R/ (7, 13), it proved possible also to isolate the oxidation product [CF3CC12NSC12 (8)] and an oligomer of the nitrile [(NCNSOF2)3 (14)]. Dechlorination of 7 with Hg gives the corresponding di-and tri-sulphides (CF3C(Cl) = N-)2Sa; (9, 10, x — 2, 3). Crystals of (14) are triclinic with a = 1133.6(5), b = 1332.6(5), c = 1715.1(8) pm, a = 109.31(3), ß = 105.30(3), y = 97.84(3)° at 170 K, Z = 8, space group P I. The structure was refined to R = 0.028 for 8290 diffractometer data with F > 4cr(F). The four crystallo-graphically independent molecules adopt similar unsymmetrical conformations. N-Sulphenylacetimidoyl halides of the type RC(X)=N-S-Y are important in preparative chem-istry for several reasons: (a) When Y is a halogen, it may be readily exchanged, leading to a chemistry analogous to that of the perhaloalkylsulfenylhalides RhaiSCl [1, 2]. Examples of such substitution reac-tions have already been reported [2, 3], (b) When the substituent X on the triply-coordinated carbon is a halogen, the -M effect of the imino-nitrogen facilitates nucleophilic attack. Hard nucleophiles (fluoride, alcohols, amines) tend to replace X [4], soft nucleophiles the sulphur-substituent Y. (c) The >C=N-S-system may be regarded as a shortened diene, in which the second double bond is replaced by the oxidisable sulphur atom; instead of the usual 1,4-addition this results in 1,3-addition with simul-taneous oxidation of the sulphur [5]. One of the simplest examples of this class of com-pounds , chlorosulphenylchloroformylimidoylchloride may be prepared in several ways; the synthesis [6] from C1CN and SC12 opens a general route to the N-sulphenylimidoyl derivatives [4, 7-9]: C1CN + SC12 C1S-N=CC12 1 RCN + R'SCl -> R'S-N=CC1R 2 * Reprint requests to Prof. R. Mews. 0340-5087/83/0400-0454/$ 01.00/0 We report here an investigation of the corresponding addition of CF3SCI and SC12 to the fluorinated nitriles N = C-CF3, N = C-NSF2 and N = C-NSOF2. Experimental | | |
Reference
| Z. Naturforsch. 38b, 454—459 (1983); eingegangen am 8. November 1982 | | |
Published
| 1983 | | |
Keywords
| Crystal Structure, Perfluoromethanesulphenylformylimidoylchlorides, N-Sulphenylchlorides, 1, 3, 5 -Triazenes | | |
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| default:Reihe_B/38/ZNB-1983-38b-0454.pdf | | | Identifier
| ZNB-1983-38b-0454 | | | Volume
| 38 | |
87 | Author
| H. W. Roesky, D. Amirzadeh-Asl | Requires cookie* | | Title
| Preparation and Reactions of Bicyclic Compounds with a Phosphorus-Phosphorus-Bond  | | | Abstract
| The reaction of N,N'-dimethyl-N,N'-bis(trimethylsilyl)urea with PCI3 leads to the bicyclic compound OP2[MeNCONMe]2 (3) with a direct phosphorus-phosphorus bond and to the bicycle MeNP2[MeNCONMe]2 (4). 3 reacts with tetrachloro-o-benzoquinone (TOB) to yield the spirocycle CeCl^tMeNCONMe^PaO (5) with a A 4 P-A 5 P-bond. The Lewis acids SbCls and SnCLj react with 3 to give the adducts 6 and 7. The reactions of 3 with the metal carbonyls Fe2(CO)9, Cr(CO)5THF and Cr(CO)4C7Hx lead to the metal complexes 8-10. The compounds were characterized on the basis of 31 P NMR and mass spectra. Kürzlich haben wir gezeigt, daß Reaktionen von disilylierten Harnstoffen mit Dichlorphosphanen, | | |
Reference
| Z. Naturforsch. 38b, 460—464 (1983); eingegangen am 14. Dezember 1982/27. Januar 1983 | | |
Published
| 1983 | | |
Keywords
| 31 P NMR, Metal Complexes, Oxidative Addition | | |
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| default:Reihe_B/38/ZNB-1983-38b-0460.pdf | | | Identifier
| ZNB-1983-38b-0460 | | | Volume
| 38 | |
88 | Author
| DavidW. Allen, LorraineA. March, IanW. Nowell, Sheffield Sil, Great Britain, JohnC. Tebby | Requires cookie* | | Title
| The Chemistry of Heteroarylphosphorus Compounds, Part 16. + An X-Ray Structural Study of (2-Thienyl)bis(2,2'-biphenylylene)phosphorane. A Comparison with Related Methyl and Aryl bis(2,2'-biphenylylene)- spirophosphoranes  | | | Abstract
| Spirophosphorane Structure, Apicophilicity of Heteroaryl Groups Crystals of the title compound are monoclinic, a= 18.9 93 (11), b = 8.757(5), c= 13.267(8) A, ß = 106.60(5)°, Z = 4 in space group Cc (Cs 4 , No. 9). The structure was determined by Patterson and electron-density methods and refined by least squares techniques to R — 0.081, R' = 0.085 for 1293 independent reflections classified as observed. The molecule is found to adopt an almost regular trigonal bipyramidal geometry in which the two biphenylylene units span apical-equatorial positions and the 2-thienyl group occupies the remaining equatorial site. The 2-thienyl group, which is disordered, does not lie in the equatorial plane, and there is no indication of C2p-i P3d.-t interactions between the heteroaryl group and phosphorus. The steric requirements of the 2-thienyl group appear to be comparable with those of methyl and phenyl groups in bis(2,2'-biphenylylene)spiro-phosphoranes. | | |
Reference
| Z. Naturforsch. 38b, 465—469 (1983); received October 18/December 6 1982 | | |
Published
| 1983 | | |
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| default:Reihe_B/38/ZNB-1983-38b-0465.pdf | | | Identifier
| ZNB-1983-38b-0465 | | | Volume
| 38 | |
89 | Author
| W. Kalz, H. Homborg | Requires cookie* | | Title
| Eisen(III)phthaloeyanine  | | | Abstract
| Darstellung und spektroskopische Charakterisierung von [Fe(OR)2Pc(—2)]~ (R = H, CH3, C2H5, (CH3)2CH, (CH3)3C), (FePc(—2))20 und FeXPc(—2) (X = F, Cl, Br, I) Iron(III)phthalocyanines: Preparation and Spectroscopic Characterisation of [Fe(OR)2Pc(—2)] -(R = H, CH3, C2H5, (CH3)2CH, (CH3)3C), FePc(—2))20 and FeXPc(—2) (X = F, Cl, Br, I) Bis-hydroxo-iron(III)phthalocyanine, Vibrational Spectra, UV-VIS Spectra, Iron (II I)phthalocy anines The preparation of bis-hydroxophthalocyaninatoferrate(III) and of some of the bis-alkoxo-analogues is described. In the presence of a small excess of OR -(R = H, CH3, C2H5, (CH3)2CH, (CH3)3C) these complexes are stable in most common non-polar solvents and can be isolated as analytically pure bis-triphenylphosphiniminium-(PNP)-salts. Solutions of these complexes react immediately with water and acids. Thus hydrolysis is an easy way to prepare (u-oxo-bis-phthalocyaninatoiron(III). The reaction with mineral acids HX (X = F, Cl, Br, I) precipitates the pure pentacoordinated halogenophthalocyaninatoiron-(III). The electronic absorption spectra have been measured. Besides the typical inner-ligand n-n*-transitions additional bands are observed at ~ll,5kK (CT1) and ~20kK (CT 2). These bands are of medium intensity only for FeXPc(—2) (X = Cl, Br, I) especially in the solid state spectra and are probably associated with ligand-to-metal-charge-transfer(CT)-transitions mainly of the Pc-^ Fe-type but partially mixed with X-^-Fe. CT 1 and CT2 are assigned to (ai),T -> (e,ai)d respectively. This is confirmed by the resonance Raman spectra. On excitation within the range of the CT 2 electronic transition some in-plane stretching-(1595 and 1550 cm -1) and out-of-plane deformation vibrations (350 and 290 cm -1) of the macrocycle as well as the Fe-X-stretching vibrations are resonance Raman enhanced. Combination bands of Fe-X-with Pc-vibrations give strong evidence for coordination of the halide to an axial position of the iron centre. As expected for C4V point symmetry the Fe-X vibrations are IR active, too (i>(Fe-X) for X = F: 475; Cl: 303; Br: 221; I: 193 cm -1). The Fe-0 stretching vibration (axg) is only observed in the reso-nance Raman spectrum of PNP[Fe(OH)2Pc(—2)] at 495 cm -1 . As a consequence of the strong antiferromagnetic coupling the IR and resonance Raman spectra of (FePc(—2))20 resemble those of closed shell ions. The IR absorption at 822 cm -1 is assigned to the anti-symmetric (a2u) (Fe-O-Fe) deformation mode. | | |
Reference
| Z. Naturforsch. 38b, 470—484 (1983); eingegangen am 18. November 1982 | | |
Published
| 1983 | | |
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| default:Reihe_B/38/ZNB-1983-38b-0470.pdf | | | Identifier
| ZNB-1983-38b-0470 | | | Volume
| 38 | |
90 | Author
| Günter Schmid, Roland Boese | Requires cookie* | | Title
| Azaborolinyl Complexes, IX [1] The Crystal and Molecular Structures of Two Isomers of Bis(l-ter£-butyl-2-methyl-??-l,2-azaborolinyl)cobalt  | | | Abstract
| The crystal and molecular structures of two isomers of bis(l-£er£-butyl-2-methyl-??-l,2-azaborolinyl)cobalt have been determined by single-crystal X-ray diffraction methods. Isomer 1 shows a clockwise, isomer 2 an anti-clockwise conformation of the azaborolinyl rings. In both compounds the azaborolinyl rings have staggered orientations with opposite positions of the tferi-butyl groups. The rings in 1 and 2 are slipped so that the three ring carbon atoms are closer to the cobalt atom than the BN groups. The staggered orientation of the ligands in 2 is probably due to a packing effect, as in similar sandwich complexes the anti-clockwise conformers show eclipsed orientation. | | |
Reference
| Z. Naturforsch. 38b, 485—492 (1983); eingegangen am 12. November 1982 | | |
Published
| 1983 | | |
Keywords
| Azaborolinyl Sandwich Complexes, Cobalt, Isomers, X-Ray | | |
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| default:Reihe_B/38/ZNB-1983-38b-0485.pdf | | | Identifier
| ZNB-1983-38b-0485 | | | Volume
| 38 | |
92 | Author
| E. L. Michelotti, E. L. Sanchez+ | Requires cookie* | | Title
| Stereospecific Synthesis of 4,8-Dimethylspiro(4,5)-deca-7-ene-l,6-dione A Synthetic Route to the Acoranes  | | | Abstract
| A stereospecific synthesis of 4,8-dimethylspiro(4,5)-deca-7-ene-l,6-dione from 4,7-di-methylcoumarine in high yield is reported. The configuration of this product is established according to its ill NMR and 13 C NMR data. | | |
Reference
| Z. Naturforsch. 38b, 497—500 (1983); received October 19 1982 | | |
Published
| 1983 | | |
Keywords
| Spirocyclisation, Acoranes, Polyphosphoric Acid | | |
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| default:Reihe_B/38/ZNB-1983-38b-0497.pdf | | | Identifier
| ZNB-1983-38b-0497 | | | Volume
| 38 | |
93 | Author
| MichaelC. Böhm, Rolf Gleiter, Waldemar Adam, Nozomu Narita | Requires cookie* | | Title
|  | | | Abstract
| Lone-pair -Lone-pair Interaction, Semiempirical Calculations The He(I) photoelectron spectra of the five-membered and six-membered peroxylactones 1 and 2 have been recorded and are analyzed on the basis of MINDO/3 calculations. A strong destabilization of the peroxo w-combination due to the adjacent carbonyl group is found. In 2 the usual peroxide sequence (n_ on top of n_) is reversed. | | |
Reference
| Z. Naturforsch. 38b, 501—503 (1983); received November 12 1982 | | |
Published
| 1983 | | |
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| default:Reihe_B/38/ZNB-1983-38b-0501.pdf | | | Identifier
| ZNB-1983-38b-0501 | | | Volume
| 38 | |
95 | Author
| H. Budzikiewicz, U. Hildebrand, W. Ockels, M. Reiche, K. Taraz | Requires cookie* | | Title
| Weitere aus dem Kulturmedium von Pseudomonas putida isolierte Pyridinderivate -Genuine Metaboliten oder Artefakte ? [1] Further Pyridine Derivatives Isolated from the Culture Medium of Pseudomonas putida - Genuine Metabolites or Artefacts ? [1]  | | | Abstract
| From the culture medium of Pseudomonas putida after treatment with CH2N2 besides the expected Pyridine-2,6-di(monothiocarboxylic acid)-di-S-methyl ester a series of pyridine derivatives could be isolated which could be shown to be artefacts formed from pyridine-2,6-di(monothiocarboxylic acid). | | |
Reference
| Z. Naturforsch. 38b, 516—520 (1983); eingegangen am 18. November 1982 | | |
Published
| 1983 | | |
Keywords
| Pyridine Derivatives, Bacterical Metabolites, Pseudomonas putida, Thiocarboxylic Acid Chemistry | | |
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| default:Reihe_B/38/ZNB-1983-38b-0516.pdf | | | Identifier
| ZNB-1983-38b-0516 | | | Volume
| 38 | |
97 | Author
| HeinzDieter Lutz, Willi Buchmeier, Bernward Engelen | Requires cookie* | | Title
| Crystal Structure of Lead Sulfite  | | | Abstract
| The crystal structure of orthorhombic PbSOß (Pnma, Z = 4, a = 790.3(1), b = 548.8(1), c = 680.2(1) pm) has been determined using single crystal X-ray diffraction data (final R for 663 reflections with I > 2<r(I) = 0.052). The para-meters of the atoms in the asymmetric unit are: Pb(4c) 0.. The sulfite ion has S-O distances of 149.4(7) and 153.7(5) (twice) pm. The Pb-0 distances of the edge-connected Pb-0 7 polyhedra (distorted mono-capped trigonal prism) range from 253.4(5) to 284.8(5) pm. The structure is closely related to that of PbS04. | | |
Reference
| Z. Naturforsch. 38b, 523—525 (1983); eingegangen am 16. Dezember 1982 | | |
Published
| 1983 | | |
Keywords
| Lead Sulfite, Crystal Structure, Sulfite | | |
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| default:Reihe_B/38/ZNB-1983-38b-0523_n.pdf | | | Identifier
| ZNB-1983-38b-0523_n | | | Volume
| 38 | |
99 | Author
| Achim Müller, Winfried Hellmann, Uwe Schimanski, Rainer Jostes, WilliamE. Newton | Requires cookie* | | Title
| On the Central Role of Sulfur in Multi Metal Aggregates with Different Electron Populations: [S2WS2CoS2WS2]' 1 - (n -2, 3)  | | | Abstract
| The hetero metal sulfur aggregates [Co(WS4)2] n ~ (with variable electron popula-tion: n = 2, 3) could be isolated as salts and characterized by physical measurements (in-cluding X-ray structure analysis). Experimental and theoretical investigations show that due to a strong metal -> ligand electron delocalisation WS4 2-(like M0S4 2 -) is a non-innocent ligand and that the additional charge upon reduction is located mainly at the S atoms of the ligand system. | | |
Reference
| Z. Naturforsch. 38b, 528—529 (1983); eingegangen am 12. November 1982 | | |
Published
| 1983 | | |
Keywords
| Preparation, Crystal Structure, Molecular Structure, Electronic Structure, Thioanions | | |
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| default:Reihe_B/38/ZNB-1983-38b-0528_n.pdf | | | Identifier
| ZNB-1983-38b-0528_n | | | Volume
| 38 | |
100 | Author
| Michael Angrick | Requires cookie* | | Title
|  | | | Abstract
| The reaction of aniline with 2,3-O-isopropyl-idene-D-glyceraldehyde supplies the dimeric form of the expected Schiff's base which may serve as a model for the initial step of the Mail-lard reaction. | | |
Reference
| Z. Naturforsch. 38b, 530 (1983); received November 11. 1982 Maillard Reaction | | |
Published
| 1983 | | |
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| default:Reihe_B/38/ZNB-1983-38b-0530_n.pdf | | | Identifier
| ZNB-1983-38b-0530_n | | | Volume
| 38 | |
|