An
efficiently scalable synthesis of key intermediate toward mirabegron
has been developed via a mixed anhydride method, employing PivCl instead
of EDCI and HOBt. The developed process produced (R)-2-hydroxy-N-(4-nitrophenethyl)-2-phenylacetamide
(10) in 91.5–92.3% yield and >99.0% HPLC purity
under mild conditions. During this process, a side reaction induced
by triethylamine hydrochloride was discovered and investigated, which
was ultimately avoided by executing the reaction in a biphasic solvent
system.
A multistep heat treatment process consisting of intercritical tempering between quenching and conventional tempering contributed to the development of a ferrite-martensite dual-phase structure in a Ni-and Cu-containing high-strength low-alloy steel. By using electron backscatter diffraction and scanning transmission electron microscopy, the microstructures were found to have an elongated lathlike morphology with carbide and Cu precipitates located especially at the boundaries of ferrite and martensite crystals. Atom probe tomography reveals at atomic scale the existence of solute-diluted ferrite and solute-rich martensite, and the later phase was considered to be transformed from the reverse austenite that was formed during intercritical tempering. Cu precipitation greatly correlates with the microconstituents, resulting in different distributional characteristics of Cu precipitates within these two phases and at their boundaries. It is a promising process to utilize Cu precipitation strengthening and phase transformation toughening simultaneously in alloy steels.
β-Nb is a typical second phase in Zr-Nb-based alloys used as fuel claddings in water-cooled nuclear reactors. The segregation of alloying element Fe may affect the corrosion resistance of Zr-Nb-based alloys. In this work, the Fe segregation at the interface between β-Nb phase and α-Zr matrix in Zr-2.5Nb alloy was studied using atom probe tomography and focused ion beam. The results suggested that the Fe concentration was much lower than Nb concentration in α-Zr matrix, while Fe selectively segregated at the β-Nb/α-Zr phase interface, leading to a Fe concentration peak at some interfaces. The peak Fe concentration varied from 0.4 to 1.2 at.% and appeared at the position where Zr concentration was approximately equal to Nb concentration. The selective segregation of Fe should be affected by the heat treatment and structure defects induced by cold rolling.
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