Synthesis of AIMCM-41 mesoporous molecular sieves with high stability

Mesoporous molecular sieves AIMCM-41 were synthesized by static hydrothermal crystallization using cetyltrimethylammonium bromide as template, water glass as silica source and pseudoboehmite as aluminum source. The XRD results showed that the prepared AlMCM-41 mesoporous molecular sieves had high relative crystallinity and long-range order. The relative crystallinity was greater than 27% after calcination at 900 ℃ for 2 hours and was still greater than 14% after ageing in steam at 800 ℃ for 2 hours. The results indicated that both thermal and hydrothermal stabilities of the mesoporous molecular sieves AIMCM-41 were good.

Identification, synthesis and characterization of process related impurities of benidipine hydrochloride, stress-testing/stability studies and HPLC/UPLC method validations

Benidipine hydrochloride, used as an antihypertensive agent and long-acting calcium antagonist, is synthesized for commercial use as a drug substance in highly pure form. During the synthetic process development studies of benidipine, process related impurities were detected. These impurities were identified, synthesized and characterized and mechanisms of their formation were discussed in detail. After all standardization procedures, they were used as reference standards for analytical studies. In addition, a separate HPLC method was developed and validated for detection of residual 1-benzylpi- peridin-3-ol （Ben-2）, which is used during benidipine synthesis and controlled as a potential process related impurity. As complementary of this work, stress-testing studies of benidipine were carried out under specified conditions and a stability-indicating UPLC assay method was developed, validated and used during stability studies of benidipine.

Preparation and characterization of H_4SiW_(12)O_(40)@MIL-100(Fe) and its catalytic performance for synthesis of 4,4'-MDA

The catalytic performance of co mmonly used heteropolyacids （H3PW12O40, H4SiW12O40 and H3PMO12O40 synthesis of 4,4＇-methylenedianiline （4,4＇-MDA） from aniline and formaldehyde was evaluated and the result showed that H4SiW12O40 with moderate acid strength exhibited the best catalytic performance. Then HaSiW12O40@MIL-100（Fe） was prepared by encapsulating H4SiW12O40 within the pores of MIL-100（Fe） to facilitate its recovery and reuse. The prepared H4SiW12O40@MIL-100（Fe） was characterized by means of FT-IR, N2 adsorption-desorption, XRD, TG and then the catalytic performance was evaluated. The result showed that H4SiW12O40 was highly dispersed in the pores of MIL-100（Fe）, and both the Keggin structure of HaSiW12O40 and the crystal skeleton structure of MIL-100（Fe） could be effectively/preserved. Furthermore, H4SiW12O40@ MIL-100（Fe） showed excellent catalytic performance under the following reaction conditions： a molar ratio of aniline to formaldehyde = 5, a mass ratio of catalyst to formaldehyde = 1.2, a reaction temperature of 120 ℃ and a reaction time of 6 h. Under the above reaction conditions, the conversion of aniline was 41.1%, and the yield and selectivity of 4,4＇-MDA were 81,6% and 79.2%, respectively. Unfortunately, an appreciable loss in the catalytic activity of the recovered H4SiW12O40@MIL-100（Fe） was observed because of the blocking of the pores and the change of the acidity resulted from the adsorption of alkaline organics such as aniline and 4,4＇-MDA. The adsorbed alkaline organics could be cleaned up when the recovered catalyst was washed by methanol and DMF. Then the catalyst was effectively reused up to three cycles without much loss in its activity.

Hydrothermal Synthesis and Visible-light Photocatalytic Activities of SnS_2 Nanoflakes

SnS2 nanoflakes were successfully synthesized via a simple hydrothermal process. The as-prepared SnS2 samples were characterized by X-ray diffraction（XRD）, scanning electron microscopy（SEM）, nitrogen adsorption-desorption isotherms, and UV-vis diffuse reflectance spectroscopy（DRS）. The photocatalytic activities of the as-prepared SnS2 nanoflakes under visible light irradiation（λ〉420 nm） were evaluated by the degradation of rhodamine B（Rh B）. The effect of hydrothermal temperatures on the photocatalytic efficiency of as-prepared SnS2 nanoflakes was investigated. The experimental result showed that SnS2 nanoflakes synthesized at the temprature of 160 o had higher photocatalytic efficiency and good photocatalytic stability.

Synthesis and biological activities of(E)-β-farnesene analogues containing 1,2,3-thiadiazole

In order to discover novel compounds with high-activity to control aphid,a series of novel（E）-β-farnesene analogues containing 1,2,3-thiadiazole were designed and synthesized,and their structures were confirmed by IR,^1H NMR,^13C NMR,and HRMS（ESI）.The stability of representative compounds was studied by HPLC and -1H NMR techniques.Repellent activity results indicated that compounds 8h and 8j displayed 60.3%and 62.0%repellent rates,respectively.The aphicidal bioassay results showed that most analogues exhibited considerable aphicidal activity against Myzus persicae.Especially,analogues 81,8s and 8t exhibited high activity with LC50 values of 33.4 μg/mL,50.2 μg/mL and 61.8 μg/mL,respectively,which were higher than the lead compound（E）-β-farnesene,but lower than commercial insecticide pymetrozine with a LC50 of 7.1 μg/mL

Synthesis, crystal structure and thermal analysis of tetraiodo-4,4'-bi-1,2,4-triazole

Tetraiodo-4,4＇-bi-l,2,4-triazole （1） was synthesized from a reaction of iodine monochloride witb 4,4＇ bi- 1,2,4-triazole （2）, which was prepared by a transamination reaction between 4-amine-1,2,4-triazole and N,N-dimethylformamide azine dihydrochloride （3） obtained via a Vilsmeier reaction. The title compound was extensively characterized by melting point, elemental analysis, 1R, HRMS and single crystal X-ray diffraction. The single crystal X-ray structural analysis reveals that compound 1 exhibits a stable conformation with the two triazole rings being perpendicular to minimize three-dimensional steric hindrance and stacking through aromatic zr. analysis from TGA and DSC indicates that resnectivelv. Jr packing interactions between molecules. The therma compound I decomposes at 275.40 ℃ and 338.35 C