5(3)-Hydroxyisoxazolidin-3(5)-ones and 5-hydroxy-pyrazolidin-3-ones and their ring-chain tautomerism

Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 2, pp. 280–281, February, 1991.     

Synthese und Kristallstruktur von (C5H5)Mo(CO)3(AuPPh3) und [(C5H5)Mo(CO)2(AuPPh3)4]PF6

Synthesis and Crystal Structure of (C₅H₅)Mo(CO)₃(AuPPh₃) and [(C₅H₅)Mo(CO)₂(AuPPh₃)₄]PF₆ CpMo(CO)₃(AuPPh₃) is obtained by the reaction of Li[CpMo(CO)₃] with Ph₃PAuCl at ?95°C in CH₂Cl₂. It crystallizes in the monoclinic space group C2/c with a = 2625.1(7), b = 883.2(1), c = 2328.4(7) pm, β = 116.39(1)° und Z = 8. In the complex the AuPPh₃ group is coordinated to the CpMo(CO)₃ fragment with a Au? Mo bond of 271,0 pm. The Mo atom thus achieves a square pyramidal coordination with the center of the Cp ring in apical position. CpMo(CO)₃(AuPPh₃) reacts under uv irradiation with an excess of Ph₃PAuN₃ to afford the cluster cation [CpMo(CO)₂(AuPPh₃)₄]⁺. It crystallizes as [CpMo(CO)₂(AuPPh₃)₄]PF₆ · 2 CH₂Cl₂ in the orthorhombic space group P2₁2₁2₁ with a = 1553.9(1), b = 1793.8(2), c = 2809.8(7) pm und Z = 4. The five metal atoms form a trigonal bipyramidal cluster skeleton with the Mo atom in equatorial position. The Mo? Au distances range from 275.5 to 280.8 pm, and the Au? Au distances are between 281.2 and 285.6 pm.     

Photochemical reactions of (CO)2 (PPh3)MnC5H4Fe(CO)2C5H5 and (CO)2(PPh3)MnC5H4COFe(CO)2C5H5 with PPh3

Conclusions The photochemical reactions of (CO)₂(PPh₃)MnC₅H₄Fe(CO)₂C₅H₅ and (CO)₂(PPh₃)MnC₅H₄COFe(CO)₂C₅H₅ with PPh₃ gave the products of replacing the CO on the Fe atom by PPh₃: respectively (CO)₂(PPh₃)MnC₅H₄Fe (CO)(PPh₃)C₅H₅ and (CO)₂(PPh₃)MnC₅H₄COFe(CO)(PPh₃)C₅H₅.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 12, pp. 2813–2815, December, 1977.     

Synthesis of 3-amino-5-nitrobenzaldehyde oxime and its conversion into 3,4-bis(3-amino-5-nitrophenyl)furoxan and isomeric 3(4)-(3-amino-5-nitrophenyl)-4(3)-nitrofuroxans

The oxime of the hitherto unknown 3-amino-5-nitrobenzaldehyde was synthesized by the reaction of 3-amino-5-nitrobenzaldehyde phenylhydrazone with excess of (NH₂OH)₂·H₂SO₄. The oxime obtained was used as the starting compound for the synthesis of novel diaryl- and arylnitrofuroxans. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 12, pp. 2232–2235, December, 1997.     

Synthesen von 3-Imidazolin-thionen-(5)

Zusammenfassung Es wird über die Darstellung neuer 2-Methyl-2,4-diaryl-3-imidazolin-thione-(5) berichtet. Sie entstehen bei Einwirkung von Ammoniak und Schwefel im Überschuß auf kernsubstituierte Acetophenonderivate bzw. acetylierte Heterocyclen in methanol. Lösung im Raumtemperaturbereich.

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The preparation of new 2-methyl-2,4-diaryl-3-imidazolin-thions-(5) is reported. These compounds are formed when ammonia und sulphur in excess react with nucleus substituted acetophenone derivatives or with acetylated heterocycles in methyl alcohol solution of room temperature.

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Herrn Professor Dr.W. Langenbeck zu seinem 65. Geburtstag gewidmet.

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44. Mitt.:F. Asinger, H. Diem undW. Schäfer, Mh. Chem.95, 1391 (1964).

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DiplomarbeitG. Kriebel, Techn. Hochschule Aachen, 1963.     

Synthesis of 3(5)-(Nitroamino)-1,2,4-triazol-5(3)-carboxylic Acid and Its Ethyl Ester

Russian Journal of Organic Chemistry -     

(C_5H_9C_5H_4)_3NdBrLi(THF)_3和(C_5H_9C_5H_4)_3SmTHF的合成与结构

无水三氯化钕与环戊烷基环戊二烯钠、溴化锂(1:2:1摩尔比)反应,除去不溶物和溶剂后,产物在己烷/四氢呋喃溶剂中冷冻得到兰紫色晶体(C5H9C5H4)3NdBrLi(THF)3(配合物1)。其中心金属Nd3+的配位数为10,以η5与3个环戊二烯基相连,并通过单溴原子桥连锂原子,形成双核结构。该晶体属三斜晶系,P`1空间群。晶体学参数为a=12.048(2)、b=13.498(3)、c=13.831(3);α=104.16(3)、β=104.07(3)、γ=95.96(3); V=2083.3(7)3、Z=2、Dc=1.35Mg/m3、Mr=847.01gmol-1、F(000)=874。无水三氯化钐与环戊烷基环戊二烯钠(1:3)反应,产物在-30oC下的己烷溶剂中结晶得桔红色晶体(C5H9C5H4)3SmTHF(配合物2)。该晶体属正交晶系,Fdd2空间群。晶胞参数a=28.175(5) 、b=46.24(2)、c=9.167(4);V=11943(8)3、Z=16、Dc=1.38Mg/m3、 Mr=622.11 g·mol-1、F(000)=5136。10配位的金属Sm3+与3个环戊二烯基以η5相连,并结合一个四氢呋喃溶剂分子。     

2-Nitroguanidine Derivatives. New Synthesis of 5(3)-Substituted 3(5)-Nitroamino-1,2,4-triazoles

Russian Journal of Organic Chemistry -     

35Cl Nuclear quadrupole resonance spectra of 3(5)-aryl-5 (3)-chloro-1,2,4-triazole

The ³⁵Cl nuclear quadrupole resonance (NQR) spectra of a number of 3(5)-aryl-5(3)-chloro-1,2,4-triazoles were studied. The energically most favorable tautomeric forms of the molecules were established, and a correlation between the ³⁵Cl NQR frequencies and the _m and ₀ reaction constants of the substituents in the aromatic ring was found.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 6, pp. 837–838, June, 1982.