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A new ring transformation of 3-halo-2-azidopyridine 1-oxides. A novel synthesis of 1,2-oxazin-6-ones
Rudolph A. Abramovitch Ichiro Shinkai Berkeley W. Cue Francis A. Ragan Jerry L. Atwood 《Journal of heterocyclic chemistry》1976,13(2):415-417
The course of the thermal ring-opening and recyclization of 2-azidopyridine 1-oxides is radically altered by the presence of a 3-halo substituent. Provided the 6-position is blocked, recyclization leads to a 6-cyano-6-halo-1,2-oxazine which hydrolyzes very readily to the 6H-1,2-oxazin-6-one. The structure of 4-bromo-3-methyl-6H-1,2-oxazin-6-one so obtained was confirmed by single crystal X-ray analysis. If the 6-position is not blocked, the product undergoes a further ring opening to give (Z)-β-cyanoacrylates. 相似文献
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Jerry D. Monroe Ermek Belekov Ali Oguz Er Michael E. Smith 《Photochemistry and photobiology》2019,95(6):1473-1481
Photodynamic therapy (PDT) is a field with many applications including chemotherapy. Graphene quantum dots (GQDs) exhibit a variety of unique properties and can be used in PDT to generate singlet oxygen that destroys pathogenic bacteria and cancer cells. The PDT agent, methylene blue (MB), like GQDs, has been successfully exploited to destroy bacteria and cancer cells by increasing reactive oxygen species generation. Recently, combinations of GQDs and MB have been shown to destroy pathogenic bacteria via increased singlet oxygen generation. Here, we performed a spectrophotometric assay to detect and measure the uptake of GQDs, MB and several GQD‐MB combinations in MCF‐7 breast cancer cells. Then, we used a cell counting method to evaluate the cytotoxicity of GQDs, MB and a 1:1 GQD:MB preparation. Singlet oxygen generation in cells was then detected and measured using singlet oxygen sensor green. The dye, H2DCFDA, was used to measure reactive oxygen species production. We found that GQD and MB uptake into MCF‐7 cells occurred, but that MB, followed by 1:1 GQD:MB, caused superior cytotoxicity and singlet oxygen and reactive oxygen species generation. Our results suggest that methylene blue's effect against MCF‐7 cells is not potentiated by GQDs, either in light or dark conditions. 相似文献
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The development of improved syntheses of PPARγ-sparing,insulin sensitizing thiazolidinedione-ketones
Steven P. Tanis Jerry R. Colca Timothy T. Parker Gerald D. Artman Scott D. Larsen Robert C. Gadwood James R. Zeller 《Tetrahedron letters》2019,60(33):150931
Ketones 2 (MSDC-0160) and 3 (MSDC-0602) had been selected for clinical development, however their initial syntheses were considered suboptimal for application deep into clinical trials. Difficulties ranging from the nature of the starting material, alcohol oxidation problems, epoxide opening regioisomeric issues, and endgame ketone redox problems had been encountered. Direct ketone introduction/maintenance was desired for maximum efficiency and convergence was found to be critically dependent upon the acidity of the nucleophilic species (13, 18) and the use of pre- or post-alkylative oximino-ether/oxime protection (vide infra). Improvements in overall yield for the syntheses of 2 (MSDC-0160) and 3 (MSDC-0602) from 20% (2) and 31% (3) respectively, to 44% (2) and 59% (3) were realized. 相似文献
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William E. Hunter Jerry L. Atwood G. Fachinetti C. Floriani 《Journal of organometallic chemistry》1981,204(1):67-74
The crystal and molecular structure of (η5-C5H5)2Zr[C4(C6H5)4] has been determined by single crystal X-ray diffraction methods. The compound is isostructural with its titanium and hafnium analogues, and crystallizes in the monoclinic space group P21/n with unit cell parameters a = 13.790(5), b = 11.136(5), c = 18.692(7) », β = 92.82(4)°, and ?calc = 1.34 g cm?3 for Z = 4. Full-matrix least-squares refinement converged with a conventional R value of 0.049 for 2986 observed reflections. The metallocyclic ring is planar to within 0.05 », and the π-electron density is largely localized. The two independent ZrC(σ) bond lengths are 2.250(5) and 2.265(6) ». The ZrC(η5) distances range from 2.482(6) to 2.546(7) », and average 2.521(20) ». A comparison of zirconium- and hafnium-carbon bonds based on the data available shows that for M = Hf the MC bonds are shorter for all cases: C(sp), C(sp2), C(sp3), C(η5). 相似文献