Lansoprazole degradation is accelerated in both acidic and basic medium in water. The present investigation deals with the hydrolytic degradation of Lansoprazole. Acidic medium degradation show all known impurities an...Lansoprazole degradation is accelerated in both acidic and basic medium in water. The present investigation deals with the hydrolytic degradation of Lansoprazole. Acidic medium degradation show all known impurities and degradation products whereas basic degradation studies show new impurity which has higher molecular weight than Lansoprazole. New impurity was identified, isolated using mass based auto purification system and characterised by 1H NMR, 13C NMR, HMBC, HSQC, NOE, COSY and HRMS experiments. Isolated impurity was showing molecular weight of 467.10, molecular formula of C23H16F3N5OS and its name is 7-(3-Methyl-4-(2,2,2-trifluoroethoxy) pyridin-2-yl)-7H-benzo[4,5]imidazo[2,1-b]benzo[4,5]imidazo[2,1-d][1,3,5]thiadiazine.展开更多
La（Ⅲ）, Y（Ⅲ） complexes with diglycol aldehyde bis-arginine （H<sub>2</sub>DAAR） and tetraglycol aldehyde bislysine （H<sub>2</sub>TALY） Schiff bases were synthesized. They were character...La（Ⅲ）, Y（Ⅲ） complexes with diglycol aldehyde bis-arginine （H<sub>2</sub>DAAR） and tetraglycol aldehyde bislysine （H<sub>2</sub>TALY） Schiff bases were synthesized. They were characterized and formulated as La（H<sub>2</sub>DAAR） （NO<sub>3</sub>）<sub>3</sub>·6H<sub>2</sub>O and Y （H<sub>2</sub>TALY）（NO<sub>3</sub>）<sub>3</sub>·5H<sub>2</sub>O separately by elemental analyses. The obtained complexes were investigated in detail by high resolution solid state （HRSS） <sup>13</sup>C NMR using cross polarization, magic angle spinning （CPMAS）, and total suppression of sidebands （TOSS）techniques. The results are supported by the liquid state 2D-<sup>1</sup>H-<sup>13</sup>C COSY NMR spectra. Some new information about the splitting peaks of <sup>13</sup>C for—CH=N—group and alkene carbon bands, etc. in HRSS <sup>13</sup>C NMR spectra are given.展开更多
Leaf and stem essential oils of Lonchocarpus cyanescens Benth., (Fabaceae) were obtained by hydro-distillation, using all-glass apparatus adapted to British Pharmacopeia specifications with yields of 0.03% and 0.17% r...Leaf and stem essential oils of Lonchocarpus cyanescens Benth., (Fabaceae) were obtained by hydro-distillation, using all-glass apparatus adapted to British Pharmacopeia specifications with yields of 0.03% and 0.17% respectively. The oils were investigated by GC and GC-MS analyses. Results show seven compounds were responsible for 90.4% of leaf;eleven compounds responsible for 97.6% of stem volatile oils. Phytol (62.5%) and hexadecanoic acid (12.4%) dominate the leaf oil;octadecenoic (24.1%) and hexadecanoic acids (17.2%) are predominant in the stem oil. Phytochemical screening of stem, leaf, and root methanol extracts of Lonchocarpus cyanescens reveal presence of following seven classes of metabolites: saponin, tannin, steroid, terpenoid, cardiac glycosides, phlobatannins and flavonoids. Partitioning of methanol extract from dried leaf of it with ethylacetate gave fraction, which was chromatographed using gradient elution. TLC with high Rf was used in monitoring elution. Two white crystalline solids eluted at 5% and 10% ethylethanoate in hexane, were re-crystallized and characterized. They were subjected to Infra-Red spectra, mass spectrometry (ESI technique), 1H and 13C-NMR analyses, which confirmed they are triterpenoids. Above mentioned metabolites may be responsible for literature acclaimed bio-activities L. cyanescens display [anti-inflammatory, anti-arthritic, anti-microbial effects]. This paper presents details of above results which are new in literature.展开更多
Single crystals of 8-Hydroxyquinoline(8-HQ) and Benzophenone substituted 8-HydroxyQuinoline(B8-HQ) are grown by slow evaporation of acetone at room temperature. Coloured crystals of 8-HQ and B8-HQ with good optical qu...Single crystals of 8-Hydroxyquinoline(8-HQ) and Benzophenone substituted 8-HydroxyQuinoline(B8-HQ) are grown by slow evaporation of acetone at room temperature. Coloured crystals of 8-HQ and B8-HQ with good optical quality of dimensions 54 × 3 × 1.5 mm3 and 27 × 3 × 1 mm3 are harvested. Single crystal X-ray diffractometer was utilized to measure the unit cell parameters and to confirm the crystal structure. The presence of various functional groups in the molecule was ascertained by FTIR spectral analysis. The cut-offwavelength of 8-HQ andB8-HQwas centered at 350 and 356 nm. The functional groups in the molecule are elucidated by 1H and 13C-NMR spectral analyses. Kurtz Perry test confirms the SHG in8-HQ andB8-HQ single crystals.展开更多
Two novel coordination compounds, [Zn(L)2(OOCH)2] (1) and [Zn(L)3(OCHO)](OCHO)]·H2O (2) (where L = 2-isopropylimidazole, C6H10N2) have been prepared by reaction of 2-isopropylimidazole with zinc(II) formate at ro...Two novel coordination compounds, [Zn(L)2(OOCH)2] (1) and [Zn(L)3(OCHO)](OCHO)]·H2O (2) (where L = 2-isopropylimidazole, C6H10N2) have been prepared by reaction of 2-isopropylimidazole with zinc(II) formate at room temperature using toluene as solvent. These compounds were characterized by elemental and thermal analyses, IR, 1HNMR and 13CNMR spectroscopies, single crystal X-ray diffraction and DFT studies. The Zn centers in 1 and 2 adopt pseudo-tetrahedral coordination geometries. Compound 1 crystallizes in the monoclinic system P2/c space group whereas compound 2 crystallizes in the P-1 space group of the triclinic crystal system. Several types of hydrogen intra-/intermolecular interactions are observed in these materials and extend into a two-dimensional leaf like network in 1 and a two-dimensional lattice of rectilinear pillars in 2. Compounds 1 and 2 were also optimized and their frontier molecular orbitals, global reactivity descriptors, molecular electrostatic potential, natural bond orbitals were investigated using density functional theory (DFT). In fact the induced structural differences from complex 1 to complex 2 led to the reduction of the frontier molecular orbital energy gap by 1.338 eV and a decrease of the chemical hardness by 0.669 eV.展开更多
Fatty acids such as oleic and stearic acids having a long hydrocarbon chain are known to exist as dimers in their melt and even in a non-polar solvent. In their melt the dimers arrange longitudinally and alternately t...Fatty acids such as oleic and stearic acids having a long hydrocarbon chain are known to exist as dimers in their melt and even in a non-polar solvent. In their melt the dimers arrange longitudinally and alternately to form clusters which resemble a smectic liquid crystal. The clusters determine the liquid properties of the fatty acids such as density, viscosity and fluidity. Then, do the dimers of fatty acid having a moderate-length hydrocarbon chain construct such the clusters? In the present study the dynamic molecular behavior and assembly structure of octanoic acid in its melt and also in CCl4 solution have been investigated by the X-ray diffraction, near infrared spectroscopy, 1H-NMR chemical shift, self-diffusion coefficient and 13C-NMR spin-lattice relaxation time measurements. From these results it has been revealed that the clusters of octanoic acid exist in its melt and also in CCl4 and that the clusters in the melt disintegrate with an increase in temperature. The dissociation profile of dimers of octanoic acid into monomers in CCl4 also has been clarified.展开更多
文摘Lansoprazole degradation is accelerated in both acidic and basic medium in water. The present investigation deals with the hydrolytic degradation of Lansoprazole. Acidic medium degradation show all known impurities and degradation products whereas basic degradation studies show new impurity which has higher molecular weight than Lansoprazole. New impurity was identified, isolated using mass based auto purification system and characterised by 1H NMR, 13C NMR, HMBC, HSQC, NOE, COSY and HRMS experiments. Isolated impurity was showing molecular weight of 467.10, molecular formula of C23H16F3N5OS and its name is 7-(3-Methyl-4-(2,2,2-trifluoroethoxy) pyridin-2-yl)-7H-benzo[4,5]imidazo[2,1-b]benzo[4,5]imidazo[2,1-d][1,3,5]thiadiazine.
基金Project supported by the National Natural Science Foundation of China (Grant No. 29671026)the Natural Science Foundation of Zhejiang Province (Grant No. 296062)the Laboratory of MRAMP (Grant No. 971502)
文摘La（Ⅲ）, Y（Ⅲ） complexes with diglycol aldehyde bis-arginine （H<sub>2</sub>DAAR） and tetraglycol aldehyde bislysine （H<sub>2</sub>TALY） Schiff bases were synthesized. They were characterized and formulated as La（H<sub>2</sub>DAAR） （NO<sub>3</sub>）<sub>3</sub>·6H<sub>2</sub>O and Y （H<sub>2</sub>TALY）（NO<sub>3</sub>）<sub>3</sub>·5H<sub>2</sub>O separately by elemental analyses. The obtained complexes were investigated in detail by high resolution solid state （HRSS） <sup>13</sup>C NMR using cross polarization, magic angle spinning （CPMAS）, and total suppression of sidebands （TOSS）techniques. The results are supported by the liquid state 2D-<sup>1</sup>H-<sup>13</sup>C COSY NMR spectra. Some new information about the splitting peaks of <sup>13</sup>C for—CH=N—group and alkene carbon bands, etc. in HRSS <sup>13</sup>C NMR spectra are given.
文摘Leaf and stem essential oils of Lonchocarpus cyanescens Benth., (Fabaceae) were obtained by hydro-distillation, using all-glass apparatus adapted to British Pharmacopeia specifications with yields of 0.03% and 0.17% respectively. The oils were investigated by GC and GC-MS analyses. Results show seven compounds were responsible for 90.4% of leaf;eleven compounds responsible for 97.6% of stem volatile oils. Phytol (62.5%) and hexadecanoic acid (12.4%) dominate the leaf oil;octadecenoic (24.1%) and hexadecanoic acids (17.2%) are predominant in the stem oil. Phytochemical screening of stem, leaf, and root methanol extracts of Lonchocarpus cyanescens reveal presence of following seven classes of metabolites: saponin, tannin, steroid, terpenoid, cardiac glycosides, phlobatannins and flavonoids. Partitioning of methanol extract from dried leaf of it with ethylacetate gave fraction, which was chromatographed using gradient elution. TLC with high Rf was used in monitoring elution. Two white crystalline solids eluted at 5% and 10% ethylethanoate in hexane, were re-crystallized and characterized. They were subjected to Infra-Red spectra, mass spectrometry (ESI technique), 1H and 13C-NMR analyses, which confirmed they are triterpenoids. Above mentioned metabolites may be responsible for literature acclaimed bio-activities L. cyanescens display [anti-inflammatory, anti-arthritic, anti-microbial effects]. This paper presents details of above results which are new in literature.
文摘Single crystals of 8-Hydroxyquinoline(8-HQ) and Benzophenone substituted 8-HydroxyQuinoline(B8-HQ) are grown by slow evaporation of acetone at room temperature. Coloured crystals of 8-HQ and B8-HQ with good optical quality of dimensions 54 × 3 × 1.5 mm3 and 27 × 3 × 1 mm3 are harvested. Single crystal X-ray diffractometer was utilized to measure the unit cell parameters and to confirm the crystal structure. The presence of various functional groups in the molecule was ascertained by FTIR spectral analysis. The cut-offwavelength of 8-HQ andB8-HQwas centered at 350 and 356 nm. The functional groups in the molecule are elucidated by 1H and 13C-NMR spectral analyses. Kurtz Perry test confirms the SHG in8-HQ andB8-HQ single crystals.
文摘Two novel coordination compounds, [Zn(L)2(OOCH)2] (1) and [Zn(L)3(OCHO)](OCHO)]·H2O (2) (where L = 2-isopropylimidazole, C6H10N2) have been prepared by reaction of 2-isopropylimidazole with zinc(II) formate at room temperature using toluene as solvent. These compounds were characterized by elemental and thermal analyses, IR, 1HNMR and 13CNMR spectroscopies, single crystal X-ray diffraction and DFT studies. The Zn centers in 1 and 2 adopt pseudo-tetrahedral coordination geometries. Compound 1 crystallizes in the monoclinic system P2/c space group whereas compound 2 crystallizes in the P-1 space group of the triclinic crystal system. Several types of hydrogen intra-/intermolecular interactions are observed in these materials and extend into a two-dimensional leaf like network in 1 and a two-dimensional lattice of rectilinear pillars in 2. Compounds 1 and 2 were also optimized and their frontier molecular orbitals, global reactivity descriptors, molecular electrostatic potential, natural bond orbitals were investigated using density functional theory (DFT). In fact the induced structural differences from complex 1 to complex 2 led to the reduction of the frontier molecular orbital energy gap by 1.338 eV and a decrease of the chemical hardness by 0.669 eV.
文摘Fatty acids such as oleic and stearic acids having a long hydrocarbon chain are known to exist as dimers in their melt and even in a non-polar solvent. In their melt the dimers arrange longitudinally and alternately to form clusters which resemble a smectic liquid crystal. The clusters determine the liquid properties of the fatty acids such as density, viscosity and fluidity. Then, do the dimers of fatty acid having a moderate-length hydrocarbon chain construct such the clusters? In the present study the dynamic molecular behavior and assembly structure of octanoic acid in its melt and also in CCl4 solution have been investigated by the X-ray diffraction, near infrared spectroscopy, 1H-NMR chemical shift, self-diffusion coefficient and 13C-NMR spin-lattice relaxation time measurements. From these results it has been revealed that the clusters of octanoic acid exist in its melt and also in CCl4 and that the clusters in the melt disintegrate with an increase in temperature. The dissociation profile of dimers of octanoic acid into monomers in CCl4 also has been clarified.
