In this paper a modified two-step procedure for synthesis of N-(1-naphthyl) suecinimide (NaS) was developed, and the molecular structure of NaS was properly characterized by XRD, FT-IR, 1H NMR, DSC, etc. The resul...In this paper a modified two-step procedure for synthesis of N-(1-naphthyl) suecinimide (NaS) was developed, and the molecular structure of NaS was properly characterized by XRD, FT-IR, 1H NMR, DSC, etc. The results show that the melting point of our product is 159 ℃-160.5 ℃, and the characteristic infrared absorption band of carbonyl group splits into two peaks (1705cm^-3/1779cm^-3), which are found to be quite different from the documented data (rap 147℃ -149℃; IR C=0-1700cm^-3). Besides, photophysical spectroscopy was found to be powerful to study the molecular structure and crystal morphology of NaS compound.展开更多
Nano-NiO and bulk NiO were prepared from Ni(AC)_2·4 H_2O by coordination precipitation using aqueous ammonia and by a solid state reaction, respectively. The nickel oxide particles were characterized by X-ray Dif...Nano-NiO and bulk NiO were prepared from Ni(AC)_2·4 H_2O by coordination precipitation using aqueous ammonia and by a solid state reaction, respectively. The nickel oxide particles were characterized by X-ray Diffraction(XRD) and scanning electron microscopy(SEM). The results indicate that nano-sized NiO has a crystal phase with a standard face-centered cubic lattice structure, with a mean particle diameter of about 10 nm. The evaluation of the activity of nickel oxide nanoparticles in the catalytic hydrogenation of 7-methoxy-1-naphthylacetonitrile was carried out. The results demonstrate the efficient synthesis of the title compound by a one-pot catalytic hydrogenation and acetylation with NiO. The NiO nanoparticles displayed superior catalytic activity in the synthesis of agomelatine in the one-pot reaction.The total yield of agomelatine is over 81.8% with a purity of 99.2%, as determined by HPLC. The structure of agomelatine was confirmed by IR, MS, and 1 H NMR analysis.展开更多
Nitro MAC(French acronym for continuous atmospheric measurements of nitrogenous compounds) is an instrument which has been developed for the semi-continuous measurement of atmospheric nitrous acid(HONO). This inst...Nitro MAC(French acronym for continuous atmospheric measurements of nitrogenous compounds) is an instrument which has been developed for the semi-continuous measurement of atmospheric nitrous acid(HONO). This instrument relies on wet chemical sampling and detection using high performance liquid chromatography(HPLC)-visible absorption at540 nm. Sampling proceeds by dissolution of gaseous HONO in a phosphate buffer solution followed by derivatization with sulfanilamide/N-(1-naphthyl)-ethylenediamine. The performance of this instrument was found to be as follows: a detection limit of around 3 ppt with measurement uncertainty of 10% over an analysis time of 10 min. Intercomparison was made between the instrument and a long-path absorption photometer(LOPAP) during two experiments in different environments. First, air was sampled in a smog chamber with concentrations up to 18 ppb of nitrous acid. Nitro MAC and LOPAP measurements showed very good agreement. Then, in a second experiment, ambient air with HONO concentrations below250 ppt was sampled. While Nitro MAC showed its capability of measuring HONO in moderate and highly polluted environments, the intercomparison results in ambient air highlighted that corrections must be made for minor interferences when low concentrations are measured.展开更多
基金Natural Science Foundation of China (50273014, 29928003)Natural Science Foundation of Tianjin (03380261).
文摘In this paper a modified two-step procedure for synthesis of N-(1-naphthyl) suecinimide (NaS) was developed, and the molecular structure of NaS was properly characterized by XRD, FT-IR, 1H NMR, DSC, etc. The results show that the melting point of our product is 159 ℃-160.5 ℃, and the characteristic infrared absorption band of carbonyl group splits into two peaks (1705cm^-3/1779cm^-3), which are found to be quite different from the documented data (rap 147℃ -149℃; IR C=0-1700cm^-3). Besides, photophysical spectroscopy was found to be powerful to study the molecular structure and crystal morphology of NaS compound.
基金Funded by the Natural Science Foundation of Hubei Province(2017CFB680)the Hubei University of Science and Technology Nuclear Technology Special Project(2018-19KZ06)+1 种基金the Open Fund of the State Key Laboratory of Refractories and Metallurgy(Wuhan University of Science and Technology)of China(G201703)the Key Laboratory of Measurement and Control System for Offshore Environment,Fuqing Branch of Fujian Normal University,Fujian Province University(S1-KF1604)
文摘Nano-NiO and bulk NiO were prepared from Ni(AC)_2·4 H_2O by coordination precipitation using aqueous ammonia and by a solid state reaction, respectively. The nickel oxide particles were characterized by X-ray Diffraction(XRD) and scanning electron microscopy(SEM). The results indicate that nano-sized NiO has a crystal phase with a standard face-centered cubic lattice structure, with a mean particle diameter of about 10 nm. The evaluation of the activity of nickel oxide nanoparticles in the catalytic hydrogenation of 7-methoxy-1-naphthylacetonitrile was carried out. The results demonstrate the efficient synthesis of the title compound by a one-pot catalytic hydrogenation and acetylation with NiO. The NiO nanoparticles displayed superior catalytic activity in the synthesis of agomelatine in the one-pot reaction.The total yield of agomelatine is over 81.8% with a purity of 99.2%, as determined by HPLC. The structure of agomelatine was confirmed by IR, MS, and 1 H NMR analysis.
基金supported by EU Sixth Framework Programme (FP6) Eurochamp program (grant number 505968)EU Seventh Framework Programme (FP7) Eurochamp-2 program (grant number 228335)+2 种基金the NeoRad program from the French National Agency for Research (ANR-07-2/21-8908)the PhotoBat project from the Primequal program of the French Ministry of Environment (Primequal-project number 19599)the PhotoPaq LIFE + program (LIFE 08/ENV/F/000487 PHOTOPAQ)
文摘Nitro MAC(French acronym for continuous atmospheric measurements of nitrogenous compounds) is an instrument which has been developed for the semi-continuous measurement of atmospheric nitrous acid(HONO). This instrument relies on wet chemical sampling and detection using high performance liquid chromatography(HPLC)-visible absorption at540 nm. Sampling proceeds by dissolution of gaseous HONO in a phosphate buffer solution followed by derivatization with sulfanilamide/N-(1-naphthyl)-ethylenediamine. The performance of this instrument was found to be as follows: a detection limit of around 3 ppt with measurement uncertainty of 10% over an analysis time of 10 min. Intercomparison was made between the instrument and a long-path absorption photometer(LOPAP) during two experiments in different environments. First, air was sampled in a smog chamber with concentrations up to 18 ppb of nitrous acid. Nitro MAC and LOPAP measurements showed very good agreement. Then, in a second experiment, ambient air with HONO concentrations below250 ppt was sampled. While Nitro MAC showed its capability of measuring HONO in moderate and highly polluted environments, the intercomparison results in ambient air highlighted that corrections must be made for minor interferences when low concentrations are measured.