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81.
Temperature and pH dual stimuli responsive PCL‐b‐PNIPAAm block copolymer assemblies and the cargo release studies 下载免费PDF全文
Sachin S. Patil Prakash P. Wadgaonkar 《Journal of polymer science. Part A, Polymer chemistry》2017,55(8):1383-1396
A new atom transfer radical polymerization (ATRP) initiator, namely, 2‐(1‐(2‐azidoethoxy)ethoxy)ethyl 2‐bromo‐2‐methylpropanoate containing both “cleavable” acetal linkage and “clickable” azido group was synthesized. Well‐defined azido‐terminated poly(N‐isopropylacrylamide)s (PNIPAAm‐N3)s with molecular weights and dispersity in the range 11,000–19,000 g mol?1 and 1.20–1.28, respectively, were synthesized employing the initiator by ATRP. Acetal containing PCL‐b‐PNIPAAm block copolymer was obtained by alkyne–azide click reaction of azido‐terminated PNIPAAm‐N3 with propargyl‐terminated PCL. Critical aggregation concentration (CAC) of PCL‐b‐PNIPAAm copolymer in aqueous solution was found to be 8.99 × 10?6 M. Lower critical solution temperature (LCST) of PCL‐b‐PNIPAAm copolymer was found to be 32 °C which was lower than that of the precursor PNIPAAm‐N3 (36.4 °C). The effect of dual stimuli viz . temperature and pH on size and morphology of the assemblies of PCL‐b‐PNIPAAm block copolymer revealed that the copolymer below LCST assembled in spherical micelles which subsequently transformed to unstable vesicles above the LCST. Heating these assemblies above 40 °C led to the precipitation of PCL‐b‐PNIPAAm block copolymer. Whereas, at decreased pH, micelles of PCL‐b‐PNIPAAm copolymer disintegrate due to the cleavage of acetal linkage and precipitation of hydrophobic hydroxyl‐terminated PCL. The encapsulated pyrene release kinetics from the micelles of synthesized PCL‐b‐PNIPAAm copolymer was found to be faster at higher temperature and at lower pH. © 2016 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2017 , 55 , 1383–1396 相似文献
82.
Enantiomeric separation of a melatonin agonist Ramelteon using amylose-based chiral stationary phase
Sachin D. Patil Nandkumar Khandekar Gajanan B. Kasawar K.A. Shaikh 《Arabian Journal of Chemistry》2013,6(1):103-109
A new simple isocratic chiral liquid chromatographic method was developed for the enantiomeric purity of Ramelteon[(S)-N-[2-(1,6,7,8-tetrahydro-2H-indeno[5,4-b]furan-8-yl) ethyl]-propionamide], a melatonin agonist in bulk drugs. The chromatographic separation was achieved on Chiralpak AD-H, 250 mm × 4.6 mm, 5 μm column using a mobile phase system consisting of n-hexane, ethanol and methanesulfonic acid in the ratio of 900:100:0.1 (v/v/v). The mobile phase was pumped on the column at the flow rate of 1 mL min?1. Addition of methane sulfonic acid in the mobile phase enhanced chromatographic efficiency and resolution between the enantiomers. The resolution between the enantiomers was found to be more than four. The developed method was subsequently validated and proved to be accurate and precise. The experimentally established limit of detection and quantification of (R)-enantiomer were found to be 25.5 and 77.2 ng ml?1, respectively, for 20 μl injection volumes. The percentage recovery of (R)-enantiomer was ranged from 98.5 to 101.9 in bulk drug samples of Ramelteon. The stability of Ramelteon sample in analytical solution was checked for about 48 h at room temperature and was found to be stable for about 48 h. The proposed method was found to be suitable and accurate for the quantitative determination of (R)-enantiomer in drug substance. 相似文献
83.
R. Nageswara Rao Dhananjay D. Shinde Sachin B. Agawane 《Biomedical chromatography : BMC》2009,23(6):563-567
A simple and rapid reversed‐phase HPLC method for determination of rifaximin in rat serum and urine was developed. Separation of rifaximin from biological matrix was achieved by direct injection of rat serum and urine onto a restricted‐access medium, Supelco LC‐Hisep, a shielded hydrophobic stationary phase, using acetonitrile:water:acetic acid (18:82:0.1 v/v/v) as a mobile phase. The linear range was 0.10–20 µg/mL (r2 > 0.999, n = 6), intraday and interday variation was <6.10%. The limits of detection and quantification were 0.03 (signal‐to‐noise ratio >3) and 0.10 µg/mL (signal‐to‐noise ratio >10), respectively. The method was successfully applied to pharmacokinetic studies of rifaximin after an oral administration to rats. Copyright © 2008 John Wiley & Sons, Ltd. 相似文献
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Shrikant B. Kanawade Shivaraj P. Patil Prashant S. Nikam Sachin A. Gangurde Madhukar N. Jachak Raghunath B. Toche 《Journal of heterocyclic chemistry》2012,49(2):363-369
o‐Aminothiophene dicarbonitrile 1 on neat reaction with cyclic ketones in anhydrous ZnCl2 yielded mixture of fused aminopyridine 3 and iminospirooxazine 4 derivatives. Similarly, pyrimidine derivatives 5 and 8 were obtained by the reaction of this intermediate 1 with formic acid and DMF‐DMA followed by hydrazine hydrate, respectively. The reaction of o‐amino‐thiophene dicarboxamide 2 at ambient temperature with cyclic ketones yielded spiropyrimidine 10 as a sole product in quantitative yield. The regioselective anellated pyrimidine 9 , 11 , and dihydropyrimidine 12 derivatives were also obtained by the reaction with aromatic aldehydes in presence of piperidine and iodine respectively. J. Heterocyclic Chem., (2012). 相似文献
87.
Sachin D. Pardeshi Bhausaheb N. Patil Prashant Patil Atul C. Chaskar 《Tetrahedron letters》2019,60(47):151250
A convenient Pictet-Splengler approach for the synthesis of substituted pyrrolo[1,2-a]quinoxalines from aryl amine and 1-(2-aminoaryl)-pyrrole has been developed. This is the first domino protocol involving formation of benzaldehyde as an intermediate from benzyl amines and benzyl alcohols using 1,2-DNB as an oxidant, followed by its endo cyclization with 1-(2-aminophenyl)-pyrrole to furnish the pyrrolo[1,2-a]quinoxalines. Notably, this procedure exhibits good functional group tolerance as well as good to moderate yield of pyrrolo[1,2-a]quinoxaline. 相似文献
88.
A series of differently substituted Chugaev‐type palladium bis(acyclic diaminocarbene) complexes was screened to identify the most active catalyst for Mizoroki–Heck coupling reactions of aryl bromides with styrene. The best catalyst, which contains three methyl groups on the bis(carbene) ligand, gives excellent coupling yields at 120 °C for both activated and deactivated aryl bromides. However, activity with aryl chlorides is limited to electron‐deficient examples. The optimized catalyst demonstrates limited air and moisture stability, giving reduced yields in couplings of activated aryl bromides in open‐flask conditions. The modular synthesis of this class of catalysts should allow further fine‐tuning of activity in Mizoroki–Heck and related coupling reactions. Copyright © 2012 John Wiley & Sons, Ltd. 相似文献
89.
Intramolecular cyclopropanation of alkenes occurs thermally with iodonium ylides in the absence of conventional metal catalysts such as Rh(II) and Cu(II). In rigid molecular systems conversions are near quantitative. A mechanism is proposed involving formal 2+2 cycloaddition followed by reductive elimination of PhI to yield the cyclopropane. 相似文献
90.
Quality profile of litchi (Litchi chinensis) cultivars from India and effect of radiation processing
Sachin N. Hajare Sudhanshu Saxena Sanjeev Kumar Surbhi Wadhawan Varsha More B.B. Mishra Madan Narayan Parte Satyendra Gautam Arun Sharma 《Radiation Physics and Chemistry》2010,79(9):994-1004
Litchi (Litchi chinensis) is a non-climacteric tropical fruit. The fruit has a short shelf-life making its marketing difficult. Physical, biochemical, microbiological, and organoleptic properties of two major commercially grown Indian cultivars of litchi, ‘Shahi’ and ‘China’ were studied. The effect of gamma radiation processing and low temperature storage on the above parameters was evaluated to standardize the optimal process parameters for shelf-life extension of litchi. Physical and biochemical parameters analyzed included weight, moisture, pH, titratable acidity, texture, color, total and reducing sugar, total soluble solids, vitamin C, and flavonoid content. Weight, moisture content, and pH in the fresh fruit ranged between 21–26 g, 74–77%, and 3.7–4.4, respectively, whereas, total and reducing sugar ranged 10–15, and 10–13 g%, respectively. In ‘Shahi’ vitamin C content was found to be around 17–19 mg%, whereas, in ‘China’ it was 22–28 mg%. Flavonoid content was in the range of 26–34 μg catechin equivalents/g of fresh fruit. Total surface and internal bacterial load was around 4 and 3 log cfu/g, respectively. Surface yeast-mold count (YMC) was ~3 log cfu/g whereas internal YMC was ~2 log cfu/g. Radiation treatment reduced microbial load in a dose dependent manner. Treatment at 0.5 kGy did not significantly affect the quality parameters of the fruit. Treated fruits retained the “good” organoleptic rating during storage. Thus, radiation treatment (0.5 kGy) in combination with low temperature (4 °C) storage achieved a shelf-life of 28 days for litchi fruit. 相似文献