scholarly journals Highly Selective Synthesis of 6-Glyoxylamidoquinoline Derivatives via Palladium-Catalyzed Aminocarbonylation

Molecules ◽  
2021 ◽  
Vol 27 (1) ◽  
pp. 4
Author(s):  
Sami Chniti ◽  
László Kollár ◽  
Attila Bényei ◽  
Attila Takács
Keyword(s):  
Selective Synthesis ◽  
Single Crystal Xrd ◽  
Atmospheric Conditions ◽  
Synthetic Route ◽  
Reaction Conditions ◽  
Isolation And Characterization ◽  
Xrd Study ◽  
Optimization Study ◽  
Palladium Catalyzed

The aminocarbonylation of 6-iodoquinoline has been investigated in the presence of large series of amine nucleophiles, providing an efficient synthetic route for producing various quinoline-6-carboxamide and quinoline-6-glyoxylamide derivatives. It was shown, after detailed optimization study, that the formation of amides and ketoamides is strongly influenced by the reaction conditions. Performing the reactions at 40 bar of carbon monoxide pressure in the presence of Pd(OAc)2/2 PPh3, the corresponding 2-ketocarboxamides were formed as major products (up to 63%). When the monodentate triphenylphosphine was replaced by the bidentate XantPhos, the quinoline-6-carboxamide derivatives were synthesized almost exclusively under atmospheric conditions (up to 98%). The isolation and characterization of the new carbonylated products of various structures were also accomplished. Furthermore, the structure of three new mono- and double-carbonylated compounds were unambiguously established by using a single-crystal XRD study.

scholarly journals Isolation and Characterization of Pectin from Pumpkin (Cucurbita maxima) Waste and Its Food Application

2019 ◽  
pp. 1-9
Author(s):  
Jayani Sandarani Maddakandage Dona
Keyword(s):  
Acid Hydrolysis ◽  
Activity Index ◽  
Dry Weight ◽  
Reaction Conditions ◽  
Isolation And Characterization ◽  
Significant Difference ◽  
Food Applications ◽  
Methoxy Content ◽  
Water Holding

Pectin was extracted using the method of acid hydrolysis followed by ethanol precipitation at various reaction conditions. Effect of blanching prior to acid hydrolysis, acid types (hydrochloric and citric) and extraction time and temperature combinations were tested to maximize the yield of pectin and they were characterized by assessing physiochemical and functional properties. The feasibility of utilizing extracted pectin in food applications was evaluated. The yield of pectin ranged from 7.30 ± 0.07- 11.04 ±0.01% on a dry weight basis. The results suggested that the highest pectin content is in the fresh pumpkin peel extracted using 0.1 N hydrochloric acid at 80±5℃, 1.25 pH for 1 hour. Water holding capacity, oil holding capacity and emulsifying activity index of pumpkin pectin were 2.5 g/g of pectin (SD 0.46), 1.76 g/g of pectin (SD 0.10) and 0.29 (SD 0.01) respectively. In addition, the degree of esterification, equivalent weight, methoxy content and galacturonic acid content of extracted pectin were 67.64% (SD 0.89%), 978.35 (SD 69.88), 6.55% (SD 0.37%) and 66.46% (SD 1.19%) respectively. Sensory analysis revealed that there is no significant difference in spreadability, surface texture and chewiness of two types of jam prepared using pumpkin and commercial pectin. In conclusion, pumpkin pectin can be categorized as high methoxy pectin.

scholarly journals Detection, Isolation and Characterization of Principal Synthetic Route Indicative Impurity in Lansoprazole

2010 ◽  
Vol 7 (3) ◽  
pp. 844-848 ◽  
Author(s):  
K. S. V Srinivas ◽  
K. Mukkanti ◽  
R. Buchi Reddy ◽  
P. Srinivasulu
Keyword(s):  
Thermal Degradation ◽  
Limit Of Detection ◽  
Catalytic Degradation ◽  
Stress Conditions ◽  
Preparative Hplc ◽  
Synthetic Route ◽  
Limit Of Quantification ◽  
Isolation And Characterization

An unknown impurity in lansoprazole (2-[[[3-methyl-4-(2, 2, 2-trifluoroethoxy)-2-pyridyl] methyl] sulfinyl] benzimidazole) was detected by HPLC and was identified as des-(trifluoroethoxy) lansoprazole, an principal synthetic route indicative impurity of lansoprazole. Lansoprazole was subjected to different ICH prescribed stress conditions like hydrolysis, oxidation, photolysis and thermal degradation conditions to enrich the impurity. The impurity was enriched by using acid catalytic degradation, isolated by using preparative HPLC and characterized (FTIR, MS and NMR). Limit of Detection (LOD) and Limit of Quantification (LOQ) are found to be 0.014% and 0.035% respectively.

scholarly journals Isolation and X-ray characterization of palladium–N complexes in the guanylation of aromatic amines. Mechanistic implications

2013 ◽  
Vol 9 ◽  
pp. 1455-1462 ◽  
Author(s):  
Abdessamad Grirrane ◽  
Hermenegildo Garcia ◽  
Eleuterio Álvarez
Keyword(s):  
Aromatic Amines ◽  
Palladium Complexes ◽  
Reaction Conditions ◽  
X Ray ◽  
Palladium Catalyzed

In the context of palladium-catalyzed guanylation of anilines herein, we have been able to characterize and isolate bis(anilino) and bis(guanidino)Pd(II) complexes using reaction conditions under which stoichiometric amounts of palladium salts are used. Characterization of these palladium complexes strongly supports a mechanistic proposal for the catalytic guanylation of anilines using PdCl2(NCCH3)2 as catalyst that involves the intermediacy of these Pd(II) complexes.

The isolation and characterization of 18 equine microsatellite loci, TKY272–TKY289

2000 ◽  
Vol 31 (2) ◽  
pp. 149-149 ◽  
Author(s):  
T Tozaki ◽  
H Kakoi ◽  
S Mashima ◽  
K Hirota ◽  
T Hasegawa ◽  
...  
Keyword(s):  
Microsatellite Loci ◽  
Isolation And Characterization
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