scholarly journals Born out of Fire and Ice: Polymorph Studies of the Antiviral Famciclovir

Crystals ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 129
Author(s):  
Liana Vella-Zarb ◽  
Ulrich Baisch
Keyword(s):  
Variable Temperature ◽  
Chemical Properties ◽  
Crystal Form ◽  
X Ray Diffraction ◽  
Crystal Forms ◽  
X Ray ◽  
Physical Chemical ◽  
Diffraction Patterns ◽  
Crystalline Forms

There is much interest and focus on solid forms of famciclovir. However, in spite of the abundance of reported differences in oral bioavailability, compressibility, and other physical–chemical properties of the various crystal forms of this drug, very little precise structural analysis is available in the literature to date. The form used in the commercial formulation is the anhydrous form I. Patents and patent applications report three different anhydrous crystalline forms on the basis of unindexed powder diffraction patterns. Single-crystal and variable-temperature X-ray diffraction experiments using the commercially available anhydrous form of famciclovir were carried out and led not only to the crystal structure determination of the anhydrous form I, but also to discovery of a new crystal form of anhydrous famciclovir from powder data.

Crystal Structure Data for Efavirenz (Sustiva™) by Combined Synchrotron X-Ray Diffraction and Electron Microscopy Techniques

2001 ◽  
Vol 7 (S2) ◽  
pp. 630-631
Author(s):  
Z. G. Li ◽  
R. L. Harlow ◽  
W. Marshell ◽  
C. M. Foris ◽  
D. Murphy ◽  
...  
Keyword(s):  
Chemical Properties ◽  
Crystal Form ◽  
Transcriptase Inhibitor ◽  
Process Conditions ◽  
X Ray Diffraction ◽  
Synthetic Process ◽  
X Ray ◽  
Cell Parameters ◽  
Solvate Form ◽  
Diffraction Patterns

Efavirenz (Sustiva™) is a non-nucleoside reverse transcriptase inhibitor (NNRTI) for the treatment of HrV-infected patients and has been in the market since 1998. Efavirenz exists as three different polymorphs (Forms I, II, III) and a nonstochiometric heptane solvate (Form IV). The current synthetic process for Efavirenz yields Form IV which is converted to the desired Form I polymorph by heating. One of the concerns for any drug substance is whether a consistent crystal form is produced in order to insure consistent physical and chemical properties, as well as to safeguard pharmacokinetic profiles. The sensitivity and resolution of single-crystal x-ray diffraction, the traditional method employed to determine unit cell parameters of drug compounds in development, are limited for Efavirenz Form IV because of the small crystallite size of the material. Furthermore, Efavirenz Form IV materials, depending on the process conditions, have slightly different powder diffraction patterns in terms of intensity when collected on standard in-house diffractometers.

scholarly journals Determination of Chromite Sands Suitability for Use in Moulding Sands

2017 ◽  
Vol 17 (2) ◽  
pp. 107-110
Author(s):  
K. Stec ◽  
J. Podwórny ◽  
B. Psiuk ◽  
Ł. Kozakiewicz
Keyword(s):  
Phase Composition ◽  
High Temperature ◽  
Chemical Composition ◽  
Chemical Properties ◽  
Grinding Process ◽  
X Ray Diffraction ◽  
Scanning Microscope ◽  
Spectroscopy Technique ◽  
X Ray

Abstract Using the available analytical methods, including the determination of chemical composition using wavelength-dispersive X-ray fluorescent spectroscopy technique and phase composition determined using X-ray diffraction, microstructural observations in a highresolution scanning microscope equipped with an X-ray microanalysis system as well as determination of characteristic softening and sintering temperatures using high-temperature microscope, the properties of particular chromite sands were defined. For the study has been typed reference sand with chemical properties, physical and thermal, treated as standard, and the sands of the regeneration process and the grinding process. Using these kinds of sand in foundries resulted in the occurrence of the phenomenon of the molding mass sintering. Impurities were identified and causes of sintering of a moulding sand based on chromite sand were characterized. Next, research methods enabling a quick evaluation of chromite sand suitability for use in the preparation of moulding sands were selected.

scholarly journals Synthesis of the Modifications of Ca2SiO4 and the Determination of their Powder X-ray Diffraction Patterns

1963 ◽  
Vol 71 (806) ◽  
pp. 63-68 ◽  
Author(s):  
Goro YAMAGUCHI ◽  
Yoshio ONO ◽  
Shigeo KAWAMURA ◽  
Yoshiaki SODA
Keyword(s):  
X Ray Diffraction ◽  
X Ray ◽  
Diffraction Patterns

Identification of Different Crystalline Forms of Diatrizoic Acid

1978 ◽  
Vol 61 (1) ◽  
pp. 72-75
Author(s):  
Victor A Folen ◽  
George Schwartzman ◽  
Millard Maienthal ◽  
Wilson L Brannon
Keyword(s):  
Weight Loss ◽  
The Other ◽  
Reference Standard ◽  
Thermal Gravimetric ◽  
X Ray Diffraction ◽  
X Ray ◽  
No Weight Loss ◽  
Diffraction Patterns ◽  
Crystalline Forms ◽  
Reference Samples

Abstract Standard reference samples of diatrizoic acid gave 2 different infrared (IR) spectra, x-ray diffraction patterns, and differential thermal and thermal gravimetric curves. One form, the anhydrous acid, shows no weight loss when heated to 170°C. The other form, the dihydrate, loses 5.36% of its weight when heated from 86 to 144°C. The anhydrous diatrizoic acid is the preferred reference standard, because it has an IR spectrum and x-ray diffraction pattern suitable for identification purposes.

Tautomeric polymorphism of the neuroactive inhibitor kynurenic acid

2019 ◽  
Vol 75 (6) ◽  
pp. 793-805
Author(s):  
Dorota Pogoda ◽  
Jan Janczak ◽  
Sylwia Pawlak ◽  
Michael Zaworotko ◽  
Veneta Videnova-Adrabinska
Keyword(s):  
Solid State ◽  
Kynurenic Acid ◽  
Variable Temperature ◽  
Neurological Diseases ◽  
Crystal Form ◽  
Phase Behaviour ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray

Kynurenic acid (KYN; systematic name: 4-hydroxyquinoline-2-carboxylic acid, C10H7NO3) displays a therapeutic effect in the treatment of some neurological diseases and is used as a broad-spectrum neuroprotective agent. However, it is understudied with respect to its solid-state chemistry and only one crystal form (α-KYN·H2O) has been reported up to now. Therefore, an attempt to synthesize alternative solid-state forms of KYN was undertaken and six new species were obtained: five solvates and one salt. One of them is a new polymorph, β-KYN·H2O, of the already known KYN monohydrate. All crystal species were further studied by single-crystal and powder X-ray diffraction, thermal and spectroscopic methods. In addition to the above methods, differential scanning calorimetry (DSC), in-situ variable-temperature powder X-ray diffraction and Raman microscopy were applied to characterize the phase behaviour of the new forms. All the compounds display a zwitterionic form of KYN and two different enol–keto tautomers are observed depending on the crystallization solvent used.

scholarly journals The crystal structures of two polyamides (‘nylons’)

1947 ◽  
Vol 189 (1016) ◽  
pp. 39-68 ◽  
Keyword(s):  
Crystal Structures ◽  
Unit Cell ◽  
Chain Molecule ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cell Dimensions ◽  
C Fibre ◽  
Diffraction Patterns ◽  
Unit Cell Dimensions ◽  
Crystalline Forms

Detailed interpretations of the X -ray diffraction patterns of fibres and sheets of 66 and 6.10 polyamides (polyhexam ethylene adipamide and sebacamide respectively) are proposed. The crystal structures of the two substances are completely analogous. Fibres of these two polyam ides usually contain two different crystalline forms, α and β, which are different packings of geometrically similar molecules; most fibres consist chiefly of the α form. In the case of the 66 polymer, fibres have been obtained in which there is no detectable proportion of the β form. Unit cell dimensions and the indices of reflexions for the α form were determined by trial, using normal fibre photographs, and were checked by using doubly oriented sheets set at different angles to the X -ray beam. The unit cell of the a form is triclinic, with a — 4·9 A, b = 5·4 A, c (fibre axis) = 17·2A, α = 48 1/2º, β = 77º, γ = 63 1/2º for the 66 polymer; a = 4·95A, b = 5·4A, c (fibre axes) = 22·4A, α = 49º, β = 76 1/2º, γ = 63 1/2º for the 6.10 polymer. One chain molecule passes through the cell in both cases. Atomic coordinates in occrystals were determined by interpretation of the relative intensities of the reflexions. The chains are planar or very nearly so; the oxygen atoms appear to lie a little off the plane of the chain. The molecules are linked by hydrogen bonds between C = 0 and NH groups, to form sheets. A simple packing of these sheets of molecules gives the α arrangement.

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