Isolation and characterization of an unusually stable formamidinium-containing macrotricyclic complex of lithium ion formed during the synthesis of 14-thia-1,4,8,11-tetraaza-bicyclo[9,5,3]nonadecane

2007 ◽  
Vol 85 (7-8) ◽  
pp. 506-512 ◽  
Author(s):  
Tosha M Barclay ◽  
Alexander McAuley ◽  
S Subramanian

Using 1,3-bis(chloroacetamido)propane (5) as the common intermediate, an efficient route is described to the stepwise syntheses of 1-thia-4,8-diazacyclodecane, [10]aneN2S (8), and the pentadentate macrobicycle 17-thia-1,4,8,11-tetraazabicyclo[9,5,3]-nonadecane (11). During the investigation of the condensation of (5) with (8), with Li2CO3 used as a base the Li+ cation is carried over as the complex of the dioxo intermediate (10) and survives further reduction. Prolonged contact of these complexes with CHCl3 during cyclisation and extraction (in the presence of Li2CO3 and NaOH, respectively), leads to the formation of the complex cation [Li(4)]2+ as a byproduct in which the cationic macrocycle (4), containing a formamidinium ring, is formed through bridging of the 1,11-nitrogens in the macrobicycle (11) by a -CH= group that is derived from CHCl3. This renders the cavity in (4) too small for the inclusion of transition metal ions. Reaction of the lithium cation [Li(4)]2+ with PdCl2 yielded the trimetallic salt [(Li(4)]-PdCl2-[(Li(4)])](ClO4)4 in which two [Li(4)]2+ ions are bridged by a PdCl2 unit through coordination of the pendant thioether donors. A crystal structure of this trimetallic salt confirms the formation of [Li(4)]2+. In contrast, if triethylamine is used as a base during the cyclisation reaction leading to the formation of (11) and contact with aqueous NaOH and CHCl3 during its isolation is minimized, the formation of (4) is prevented and the yield of (11) improved.Key words: macrobicycle synthesis, lithium, formamidinium, paaladium, complex.

Author(s):  
Madhubhushan M ◽  
Seshaiah S ◽  
Chandrudu J ◽  
Sagar R ◽  
Akila CR

The common watermelon item (Citrullus lanatus) seeds were gained from castoffs verdant nourishments for use by decorating, sun ventilation and pulverizing. Light yellow-toned oil was gotten by dissolvable withdrawal using oil atmosphere and the going with traits were gotten using oil ether: pH, refractive rundown, thickness, dissolvable miscibility, coagulating temperature, fire nature, express gravity, streak point and warmth of consuming. With a shallow level of unsaturation, stepped level of smoothness, and proximity of raised degree of the sensible proportion of free unsaturated fats. The low assessment of the solidifying temperature of the oil offered a hint that the oil can be managed in various areas paying little heed to the qualification in temperature. The following level of linoleic destructive of the oil offers a hint of natural gradation of solidarity. Fatty esters are increasing expanding significance as a biodegradable swap for mineral oils. In some request regions, for example, cutting tool oil, gearbox, pressure-driven oils, and greases for raw petroleum creation, the oleochemical items are set up. Nonetheless, certain particular wellsprings of fatty esters are hitherto to be abused for this comparative reason. This exploration subsequently tests into one of the less used wellsprings of fatty esters in watermelon. The oil from the kernels demonstrations a top-notch yield presents significant utilitarian gatherings for change and thus was utilized to set up an assortment of oleochemicals which demonstrated excellence materials in contrast with the routinely utilized oils feed frameworks for oleochemicals after portrayal. The photopolymers acquired indicated piercing vinyl protons for consistent polymerize.


Peptides ◽  
2003 ◽  
Vol 24 (1) ◽  
pp. 35-43 ◽  
Author(s):  
Atsuhiro Kanda ◽  
Eiko Iwakoshi-Ukena ◽  
Kyoko Takuwa-Kuroda ◽  
Hiroyuki Minakata

2020 ◽  
Vol 44 (26) ◽  
pp. 10781-10785
Author(s):  
Vedichi Madhu ◽  
Arun Kumar Kanakati ◽  
Samar K. Das

Here we report the synthesis, isolation, and characterization of a dication salt, namely 4,6-bis(4,4′-bipyridinium)-1,3,5-triazin-2-one {12+(PF6)22−·2H2O1(PF6)2·2H2O}, and its radical cation salt, namely 4,6-bis(4,4′-bipyridinium)-1,3,5-triazin-2-one (1+˙PF6−1˙PF6).


The formation of N -glycosidic linkages of eukaryotic glycoproteins involves the assembly of a specific lipid-linked precursor oligosaccharide in the endoplasmic reticulum. This oligosaccharide is transferred from the lipid carrier to appropriate asparagine residues during protein synthesis. The protein-linked oligosaccharide then undergoes processing reactions that include both removal and addition of carbohydrate residues. In this paper we report recent studies from our laboratory on the synthesis of asparagine-linked oligosaccharides. In the first part we describe the isolation and characterization of temperature-sensitive mutants of yeast blocked at specific stages in the assembly of the lipid-linked oligosaccharide. In addition, we are using these mutants to clone the genes for the enzymes in this pathway by complementation of the temperature-sensitive phenotype. The second part deals with the topography of asparagine-linked oligosaccharide assembly. Our studies on the transmembrane movement of sugar residues during the assembly of secreted glycoproteins from cytoplasmic precursors are presented. Finally, experiments on the control of protein-linked oligosaccharide processing are described. Recent data are presented on the problem of how specific oligosaccharides are assembled from the common precursors at individual sites on glycoproteins.


Polyhedron ◽  
1994 ◽  
Vol 13 (17) ◽  
pp. 2501-2505 ◽  
Author(s):  
Edward W. Abel ◽  
Peter J. Heard ◽  
Keith G. Orrell ◽  
Michael B. Hursthouse ◽  
K.M. Abdul Malik

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