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Yagi H Ramesha AR Kalena G Sayer JM Kumar S Jerina DM 《The Journal of organic chemistry》2002,67(19):6678-6689
We describe a novel and efficient synthesis (62-84% yields) of the eight possible, diastereomerically pure, cis and trans, R and S O(6)-allyl-protected N(2)-dGuo phosphoramidite building blocks derived through cis and trans opening of (+/-)-3alpha,4beta-dihydroxy-1beta,2beta-epoxy-1,2,3,4-tetrahydrobenzo[c]phenanthrene [BcPh DE-1 (1)] and (+/-)-3alpha,4beta-dihydroxy-1alpha,2alpha-epoxy-1,2,3,4-tetrahydrobenzo[c]phenanthrene [BcPh DE-2 (2)] by hexafluoropropan-2-ol (HFP)-mediated addition of O(6)-allyl-3',5'-di-O-(tert-butyldimethylsilyl)-2'-deoxyguanosine (3) at C-1 of the epoxides. Simply changing the relative amount of HFP used in the reaction mixture can achieve a wide ratio of cis/trans addition products. Thus, the observed cis/trans adduct ratio for the reaction of DE-1 (1) in the presence of 5 equiv of 3 varied from 17/83 to 91/9 over the range of 5-532 equiv of HFP. The corresponding ratios for DE-2 (2) varied from 2/98 to 61/39 under the same set of conditions. When 1 or 2 was fused with a 20-fold excess of 3 at 140 degrees C in the absence of solvent HFP, almost exclusive trans addition (>95%) was observed for the both DEs. Through the use of varying amounts of HFP in the reaction mixture as described above, each of the eight possible phosphoramidite oligonucleotide building blocks (DE-1/DE-2, cis/trans, R/S) of the BcPh DE N(2)-dGuo adducts can be prepared in an efficient fashion. To rationalize the varying cis-to-trans ratio, we propose that the addition of 3 to 1 or 2 in the absence of solvent or in the presence of small amounts of HFP proceeds primarily via an S(N)2 mechanism to produce mainly trans-opened adducts. In contrast, increasing amounts of HFP promote increased participation of an S(N)1 mechanism involving a relatively stable carbocation with two possible conformations. One of these conformations reacts with 3 to give mostly trans adduct, while the other conformation reacts with 3 to give mostly cis adduct. 相似文献
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Rebecca J. Hopkins Rachel Symes Robert M. Sayer Jonathan P. Reid 《Chemical physics letters》2003,380(5-6):665-672
Cavity-enhanced Raman scattering is used to determine the size and composition of multicomponent ethanol/water droplets in the concentration range 7.5–19% ethanol by volume. Under the experimental conditions presented here, the integrated CERS signal from ethanol shows an exponential increase with increase in ethanol concentration when compared with the integrated intensity of the water band. The calibration is shown to be invariant with particle size over the droplet radius range 20–35 μm. In addition to providing a method for determining particle size and composition, initial studies show that the evaporation dynamics of these multicomponent droplets can be probed by CERS. 相似文献
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Rafiq Shahid Abbas Zaheer Nawaz Muhammad Alharbi Sayer Obaid 《Journal of Thermal Analysis and Calorimetry》2021,145(6):3269-3279
Journal of Thermal Analysis and Calorimetry - A numerical model is developed to study the effects of temperature-dependent viscosity on heat transfer in magnetohydrodynamic flow of micropolar fluid... 相似文献
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Franklin David Rincón Marcelo Esposito Pedro Henrique Hermes de Araújo Claudia Sayer Galo Antonio Carrillo Le Roux 《大分子反应工程》2013,7(1):24-35
Reaction calorimetry is a very useful tool to monitor exothermic polymerization reactions as it is based on the estimation of the heat generated by the reaction. The objective of this work is to analyze the performance of an unscented Kalman filter (UKF) for online monitoring of batch vinyl acetate emulsion polymerization reactions. Reactions are performed in isoperibolic and isothermal conditions. The UKF is compared to an extended Kalman filter that has a very poor performance. The results show that the UKF is able to provide good estimates for the conversion, for the reactor and jacket temperatures, for the overall heat transfer coefficient between the reaction medium and the jacket, and for the heat loss from the jacket to the surroundings.
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A review of the experimental data on a range of transition metal oxide glasses shows a strong relationship between activation energy and site spacing for glasses based on V2O5. The behaviour confirms that transport in amorphous V2O5 and vanadate glasses is by adiabatic hopping with an appreciable polaron bandwidth, while non-adiabatic hopping between isolated centres is apropriate for glasses based on most other transition metal oxides. The behaviour of vanadium is linked to the retention of a well-defined VO5? structural unit in the glass network and to optimisation of the packing of this unit within the glass. 相似文献
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The dc conductivity of semiconducting vanadium tellurite glasses of compositions in the range 50 to 80 mol% V2O5 has been measured in the temperature region 77 to 400 K. Measurements have been made on annealed samples at different annealing temperatures. Annealing the samples at temperature of about 250°C causes the appearance of a complex crystalline phase resulting in an increase of conductivity. Results are reported for amorphous samples of different compositions. The conductivity of tellurite glasses is slightly higher than the corresponding composition of phosphate glasses, but the general trend of the increase of conductivity and decrease of high temperature activation energy with increasing V2O5 content is similar in the two systems. The data have been analysed in the light of existing models of polaronic hopping conduction. A definite conclusion about the mechanics of conduction (adiabatic or nonadiabatic) is difficult in the absence of a precise knowledge of the characteristic phonon frequency v0. Adiabatic hopping is indicated for v0~1011 Hz, however this value leads to unreasonably low value for the Debye temperature θD, and higher values for v0~1013 hz satifiies the conditions for nonadiabatic hopping which appears to be the likely mechanism of conduction in V2O5TeO2 glasses. The low temperature data (< 100 K) can be fitted to Mott's variable range hopping, which when combined with ac conductivity data gives reasonable values of α, but a high value for the disorder energy. 相似文献