A convenient com. scale synthesis of 5-(4'-(substituted)-[1,1'-biphenyl]-2-yl)-1H-tetrazole, a common intermediate for so many angiotensin II receptors antagonists, has been achieved with high purity using a simple synthetic protocol.The advantage of this route includes inexpensive starting materials, mild conditions, and acceptable overall yield.The application of this synthesis is well demonstrated in com. preparation of valsartan.

International Journal of Chemical Studies

N, N-(dialkylsubstituted)-1,2-diarylethylene diamines: chemical ionization mass spectral analysis

Author: Harrod, John F. ; Reddy, Kesamreddy Ranga ; Saade, Nadim ; Reddy, Emani Vijayabhaskar

The chem. ionization mass spectra of a series of vicinal diamines (N,N,N',N'- tetraalkyl-1,2-diarylethylenediamines), Ar = Ph, or substituted Ph, (1 to 46), synthesized by a novel reductive coupling of N,N-dialkyl benzamides in the presence of organosilane and Titanium have been recorded.Accurate mass measurements were used to confirm the identity of the principal fragmentation products.It is proposed that the primary fragmentation pathway originates from an initial C(1)-C(2) bond cleavage (α-cleavage) with charge retention on the nitrogen atom of one of the fragments, followed by sequential loss of two mols. of methane (R¹R² = Me₂) or ethylene (R¹,R² = Et₂).This fragmentation pathway initially leads to a stabilized benzylidene dialkylimonium ion, which constitutes the base peak in the spectra of all of the studied compounds, except for the case of R¹R² = Ph(Me), where the base peak arises from the unimol. deamination of [M+H]⁺.The relative importance of the two principal fragmentation pathways depends strongly on the nature of the substituents on the aryl group, as also do the subsequent fragmentations.Spectra were recorded for both the meso- and rac- isomer of each compound and only minor differences were observed between the spectra of the two diastereoisomers.

International Journal of Current Research

Large scale synthesis of high purity iopamidol

Author: Reddy, Kesamreddy Ranga ; Kumar, J. V. Shanmukha ; Sunil, Lingareddy ; Reddy, Emani Vijayabhaskar

A com. scale synthesis of ultra-pure Iopamidol 1 has been achieved using a simple protocol employing with a total of 9 steps and easily isolatable intermediates.The key intermediate (S)-1-((3,5-bis-(chlorocarbonyl)-2,4,6-triiodophenyl)amino)-1-oxopropan-2-yl acetate 7 has been synthesized with high purity.The main advantages of the route include readily available inexpensive starting materials and good overall yield of 78%.The process impurities including chiral analog have been well controlled without using any resins or chiral separation techniques but with simple chromatog. grade silica treatment.The structures of all intermediates prepared were confirmed by NMR, IR and MS and HPLC anal.

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