RESUMO
The title compound, 2,6-di-amino-5-[(2-cyclo-propyl-7,8-dimeth-oxy-2H-1-benzo-pyran-5-yl)meth-yl]pyrimidin-1-ium methane-sulfonate, C19H23N4O3 +·CH3O3S-, is a salt made up from a protonated iclaprim mol-ecule and a mesylate anion. The pyrimidine and chromene units of the iclaprim mol-ecule form an orthogonal arrangement [inter-planar angle of 89.67â (6)°], and the 3-nitro-gen position of the pyrimidine ring is protonated. Four distinct N-Hâ¯O inter-actions and an additional N-Hâ¯N hydrogen bond connect iclaprim and mesylate mol-ecules to one another, resulting in an infinite hydrogen-bonded mol-ecular tape structure. The central section of the tape is formed by a sequence of fused hydrogen-bonded rings involving four distinct ring types.
RESUMO
In the title structure, 5-fluoro-3-phenyl-2-[(1S)-1-(9H-purin-6-yl-amino)-prop-yl]quinazolin-4(3H)-one (= idelalisib) tert-butanol monosolvate dihydrate, C22H18FN7O·C4H10O·2H2O, the idelalisib mol-ecule displays planar quinazoline and purine systems which are nearly perpendicular to one another. Seven distinct hydrogen-bonding inter-actions link the idelalisib, t-BuOH and water mol-ecules into a complex chain structure with the topology of a 2,3,4,5-connected 4-nodal net having the point symbol (3.4.52.62)(3.4.52.64.72)(3.5.6)(5).
RESUMO
In the salt (5α,6α)-6-[(2,5,8,11,14,17,20-hepta-oxadocosan-22-yl)-oxy]-3,14-dihy-droxy-17-(prop-2-en-1-yl)-4,5-ep-oxy-morphinan-17-ium hydrogen oxalate, C34H54NO11+·C2HO4- the polyether unit of the naloxegol cation adopts the shape of a squashed open letter 'O'. In the crystal, the hydrogen oxalate anions are linked into a chain by O-Hâ¯O hydrogen bonds. Each naloxegol unit is hydrogen bonded to three hydrogen oxalate ions via two O-Hâ¯O and one N-Hâ¯O inter-actions. The resulting hydrogen-bonded two-dimensional layer structure is 3,5-connected and has the 3,5 L50 topology.
RESUMO
The sotagliflozin molecule exhibits two fundamentally different molecular conformations in form 1 {systematic name: (2S,3R,4R,5S,6R)-2-[4-chloro-3-(4-ethoxybenzyl)phenyl]-6-(methylsulfanyl)tetrahydro-2H-pyran-3,4,5-triol, C21H25ClO5S, (I)} and the monohydrate [C21H25ClO5S·H2O, (II)]. Both crystals display hydrogen-bonded layers formed by intermolecular interactions which involve the three -OH groups of the xyloside fragment of the molecule. The layer architectures of (I) and (II) contain a non-hydrogen-bonded molecule-molecule interaction along the short crystallographic axis (a axis) whose total PIXEL energy exceeds that of each hydrogen-bonded molecule-molecule pair. The hydrogen-bonded layer of (I) has the topology of the 4-connected sql net and that formed by the water and sotagliflozin molecules of (II) has the topology of a 3,7-connected net.
RESUMO
Quality assurance and process understanding are assuming increasing importance in the production of Active Pharmaceutical Ingredients (APIs). NMR has the potential to report on physical processes, quantities, structures, and speciation as chemical reactions progress. Following the progression of chemical reactions by placing the sample in an NMR tube, one can perform a large number of useful studies that provide chemical and mechanistic insight. But this simple approach can have limitations, and we have therefore constructed an apparatus comprising a laboratory reactor coupled with an NMR flow cell. The reactor duplicates the exact reaction conditions that will apply with large-scale production. This reaction mixture is sampled and pumped to a high-resolution NMR flow cell where the spectrum is recorded through the course of the reaction. We demonstrate the utility of reaction monitoring using NMR both for simple cases where tubes can be used, and describe the design of the on-flow apparatus and highlight its utility with an example.