Synthesen mit aliphatischen Dialdehyden, XXVII [1] Eine „non-template“-Synthese zur Darstellung metallfreier 1.4.8.11-Tetraaza [14] annulen-Derivate / Syntheses with Aliphatic Dialdehydes, XXVII [1] A Non-Template Synthesis for the Preparation of Metal-Free 1,4,8,11-Tetraaza[14]annulene Derivatives

1978 ◽  
Vol 33 (9) ◽  
pp. 1012-1015 ◽  
Author(s):  
Christian Reichardt ◽  
Wolfgang Scheibelein

The reaction of 2-substituted malonaldehydes (7) with aromatic 1,2-diamines (5 or 6) in ethanol/acetic acid (10:1) leads to 6,13-disubstituted 1,4,8,11 -tetraaza[14]annulene derivatives (8 or 9) even in the absence of coordinating metal cations ("non-template" synthesis), and not to 3-substituted 1,5-benzodiazepines such as 4. Cobalt(II), nickel(II), and copper(II) complexes of the macrocyclic chelate ligands 8 and 9 have been observed by subsequent metallization with the corresponding acetates in N,N-dimethylformamide. The structures of 8-11 have been assigned mainly by their mass spectra.

Author(s):  
T E Saraswati ◽  
A O Nandika ◽  
I F Andhika ◽  
Patiha ◽  
C Purnawan ◽  
...  

2011 ◽  
Vol 236-238 ◽  
pp. 2495-2498 ◽  
Author(s):  
Xue Song Huang ◽  
Xian Zhe Lin ◽  
Mo Ting Guo ◽  
Ya Zou

The solution of piperine in multiple solvent including ethanol, acetic acid, water and HCl were investigated to extract more piperine from piper fruit. Piperine was determined by reverse phase high-performance liquid chromatography with Diamonsil column (C18,5 μm ,250 mm×4. 6 mm) at 343 nm. Experiment data were simulated by Allometric model and the formula is Z=0.9+ 4.54×10-10×x5.675+1.8029×y2.12848+2.37×10-10×x5.675×y2.12848(Z:sample solution,mol/mL,x: the percentage of ethanol’s volume, ml/100mL,y: the acetic acid in the authentic sample solution, g/100mL), the adj·R2=0.997, the comparative deviation less than 2%. These results are good in agreement with experimental data. It reveals that the model can meet the requirements of the selection and design in extracting piperine from piper fruit.


1961 ◽  
Vol 34 (2) ◽  
pp. 226-229 ◽  
Author(s):  
Kozo Hirota ◽  
Kazuo Nagoshi ◽  
Motoyoshi Hatada
Keyword(s):  

2003 ◽  
Vol 9 (3) ◽  
pp. 165-173 ◽  
Author(s):  
Magdalena Frańska ◽  
Agnieszka Zgoła ◽  
Joanna Rychłowska ◽  
Andrzej Szymański ◽  
Zenon Łukaszewski ◽  
...  

The mass spectrometric behaviour of mono- and di-carboxylated polyethylene glycols (PEGCs and CPEGCs) and carboxylated octylphenol ethoxylates (OPECs) is discussed. The tendency for ionisation (deprotonation, protonation and cationisation by alkali–metal cations) of carboxylated PEGs was compared with that of non-carboxylated analogues by using both secondary-ion mass spectrometry (SIMS) and electrospray ionisation (ESI). The fragmentation of the PEGCs and CPEGCs is discussed and also compared with their neutral analogues, PEGs. B/E linked-scan mass spectra were recorded, using secondary-ion mass spectrometry as a method for ion generation, for deprotonated and protonated molecules as well as for molecules cationised by alkali–metal cations. The fragmentation behaviour of PEGs is found to be different from that of CPEGCs, The presence of carboxyl groups may be confirmed not only by the determination of molecular weights of the ethoxylates studied, but also on the basis of the fragment ions formed. The metastable decomposition of the [OPEC-H]− ions proceeds through the cleavage of the bond between the octylphenol moiety and the ethoxylene chain and leads to the octylphenoxyl anions. It permits determination of the mass of the hydrophobic moiety of the studied carboxylated alkylphenol ethoxylate. ESI mass spectra recorded in the negative-ion mode were found to be more suitable than SI mass spectra for the determination of the average molecular weight of carboxylated ethoxylates.


1954 ◽  
Vol 32 (1) ◽  
pp. 147-153 ◽  
Author(s):  
A. C. Neish ◽  
F. J. Simpson

D-Glucose-1-C14, D-arabinose-1-C14, and L-arabinose-1-C14 were dissimilated anaerobically by Aerobacter aerogenes. The major products (2,3-butanediol, ethanol, acetic acid, lactic acid, formic acid, and carbon dioxide) were isolated and the location of C14 determined. The products from glucose were all labeled, mainly in the methyl groups, in agreement with the hypothesis that they were derived from methyl-labeled pyruvate formed by the reactions of the classical Embden–Meyerhof scheme for glycolysis. The products from both pentoses appeared to have been formed from pyruvate labeled in both the methyl and carboxyl groups with twice as much C14 in the methyl group as in the carboxyl group. This result may be explained quantitatively by a hypothesis assuming complete conversion of pentose to triose via a heptulose.


1984 ◽  
Vol 39 (2) ◽  
pp. 248-251 ◽  
Author(s):  
Lutz Grotjahn ◽  
Volker B. Koppenhagen ◽  
Ludger Ernst

Hydrogenobalam in (metal-free vitamin B12) and cupribalamin are characterized by their fast atom bombardment (FAB) mass spectra which show molecular ion and characteristic fragment ion peaks. These spectra and the high-resolution FAB mass spectrum of cobalamin (vitamin B12) show that the (M+H)+-CN-59 peak for the latter is due to loss of acetamide and not of the central cobalt atom. In the FAB mass spectrum of cupribalamin metal clusters are observed


2017 ◽  
Vol 7 (20) ◽  
pp. 4818-4822 ◽  
Author(s):  
Youming Ni ◽  
Lei Shi ◽  
Hongchao Liu ◽  
Wenna Zhang ◽  
Yong Liu ◽  
...  

Halide-free and noble metal-free pyridine-modified H-mordenites exhibit high stability and selectivity in methanol carbonylation to acetic acid.


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