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131.
[formula: see text] A novel type of palladium-catalyzed cascade cyclization-coupling reaction that proceeds with suppressed beta-hydride elimination has been found. One of the N-sulfonyl oxygens is suggested to coordinatively stabilize an alkylpalladium intermediate, thus preventing the intermediate from the usual beta-elimination. This is the first sequential palladium-catalyzed coupling reaction where the Suzuki and Heck reactions can compete. The reaction provides an efficient synthetic route to 4-methylene-3-arylmethylpyrrolidines, which are not readily available by other routes. 相似文献
132.
Yan B Collins N Wheatley J Irving M Leopold K Chan C Shornikov A Fang L Lee A Stock M Zhao J 《Journal of combinatorial chemistry》2004,6(2):255-261
We have developed a high-throughput purification system to purify combinatorial libraries at a 50-100-mg scale with a throughput of 250 samples/instrument/day. We applied an accelerated retention window method to shorten the purification time and targeted one fraction per injection to simplify data tracking, lower QC workload, and simplify the postpurification processing. First, we determined the accurate retention time and peak height for all compounds using an eight-channel parallel LC/UV/MS system, and calculated the specific preparative HPLC conditions for individual compounds. The preparative HPLC conditions include the compound-specific gradient segment for individual compounds with a fixed gradient slope and the compound-specific UV or ELSD threshold for triggering a fraction collection device. A unique solvent composition or solvent strength was programmed for each compound in the preparative HPLC in order to elute all compounds at the same target time. Considering the possible deviation of the predicted retention time, a 1-min window around the target time was set to collect peaks above a threshold based on UV or ELSD detection. Dual column preparative instruments were used to maximize throughput. We have purified more than 500 000 druglike compounds using this system in the past 3 years. We report various components of this high-throughput purification system and some of our purification results. 相似文献
133.
R.E. Benner K.U. Von Raben K.C. Lee J.F. Owen R.K. Chang B.L. Laude 《Chemical physics letters》1983,96(1):65-69
Raman scattering from Pt(CN)42? adsorbed on Pt colloids (average diameter of 16 A) is compared with the Raman signal from the same amount of Pt(CN)42? in solution. The wavelength dependence of the adsorbate Raman intensity is measured from 308 to 647 nm and compared with a Lorenz/Mie calculation of the enhancement factor for the electromagnetic field intensity on the surface of a Pt sphere as a function of sphere radius and incident wavelength. 相似文献
134.
Gong Y Xiang Y Yue B Xue G Bradshaw JS Lee HK Lee ML 《Journal of chromatography. A》2003,1002(1-2):63-70
Two bonded chiral stationary phases (CSPs), 8-aminoquinoline-2-ylmethyl- and 8-aminoquinoline-7-ylmethyl-diaza-18-crown-6-capped [3-(2-O-beta-cyclodextrin)-2-hydroxypropoxy]propylsilyl silica particles (non-porous, 1.5 microm), have been prepared and evaluated using capillary liquid chromatography at high pressures (> or = 8000 p.s.i.). High column efficiency (up to 400 000 plates m(-1)) was achieved for chiral separations. These CSPs with two recognition sites, i.e. substituted-diaza-18-crown-6 and beta-cyclodextrin combined with high chromatographic efficiency provide good resolution of a variety of enantiomers and positional isomers in relatively short times under reversed-phase conditions. After inclusion of a Ni (II) ion from the mobile phase, the positively charged crown ether-capped beta-cyclodextrin facilitates specific static, dipolar, and host-guest complexation interactions with solutes. 相似文献
135.
Dendritic molecular capsules for hydrophobic compounds 总被引:1,自引:0,他引:1
Morgan MT Carnahan MA Immoos CE Ribeiro AA Finkelstein S Lee SJ Grinstaff MW 《Journal of the American Chemical Society》2003,125(50):15485-15489
Reichardt's dye, a highly solvatochromic dye, was encapsulated within poly (glycerol succinic acid) ([Gn]-PGLSA-OH) dendrimers to investigate the interior environment of these dendritic macromolecules. The absorption maximum for the encapsulated Reichardt's dye in water was indicative of a relatively high dielectric constant present within the dye/dendrimer complex. (1)H NMR of the encapsulated complex showed the presence of aromatic protons from Reichardt's dye along with the aliphatic protons of the dendrimer. Additionally, there were substantial changes in T(1) and T(2) times of the encapsulated dye when compared with the free dye, and (1)H NOESY spectra for the complex showed a significant number of intermolecular NOE cross-peaks. These data reveal the close through-space proximity of the dye to the dendrimer and the restricted motion of the encapsulated dye. To demonstrate the potential use of these macromolecules as drug delivery vehicles, the poorly water-soluble anticancer drug 10-hydroxycamptothecin (10HCPT) was encapsulated within a carboxylated PGLSA dendrimer ([G4]-PGLSA-COONa). Cytotoxicity assays with human breast cancer cells showed a significant reduction of cell viability, demonstrating that 10HCPT retains activity upon encapsulation. 相似文献
136.
Hae‐Jeong Lee Christopher L. Soles Da‐Wei Liu Barry J. Bauer Wen‐Li Wu 《Journal of Polymer Science.Polymer Physics》2002,40(19):2170-2177
X‐ray reflectivity has been used to determine the mass uptake of probe molecules in porous thin films supported on thick silicon wafers. The adsorption occurs by capillary condensation when the films are exposed to probe vapor at controlled partial vapor pressures. The probe solvent partial pressure was varied by mixing saturated air and dry air at constant temperature or by changing sample temperature at a constant vapor concentration. Pore size distribution in the films can be calculated from the probe uptake with typical porosimetric approaches such as the application of the Kelvin equation to convert partial pressure into pore size. For illustration, the pore size distribution of three different nanoporous thin films, the primary candidate of ultra‐low‐k interlevel dielectrics in the next generation of integrated circuit chips, was determined with this technique. These samples represent different generations of low‐k dielectrics developed by industry. © 2002 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 40: 2170–2177, 2002 相似文献
137.
The neutron irradiated potassium hexacyanoferrate(III) solutions were analyzed for Fe(CN)64?, Fe(CN)63?, and Prussian blue. The retention values (1.1%) were constant throughout the pH and concentration ranges studied, and did not change with the length of irradiation. The complex behavior of the radiochemical yield of the Fe(CN)64? and Prussian blue was attributed to the competition of the various reactions involved in the irradiation. 相似文献
138.
Kazufumi Takahashi Raymond N. Castle Milton L. Lee 《Journal of heterocyclic chemistry》1987,24(4):977-979
The four acridinecarbaldehydes, namely, acridine-1-carbaldehyde, acridine-2-carbaldehyde, acridine-3-carbaldehyde, and acridine-4-carbaldehyde have been synthesized for the first time. 相似文献
139.
140.
J. S. Bradshaw N. W. Adams R. S. Johnson B. J. Tarbet C. M. Schregenberger M. A. Pulsipher M. B. Andrus K. E. Markides M. L. Lee 《Journal of separation science》1985,8(10):678-683
Contemporary methods for the synthesis of alkyl- and arylsubstituted polysiloxane stationary phases are reviewed. A new, moderately polar phase containing the 3-(4-methoxyphenyl)-propyl group is reported. 相似文献