Process Research of 1-(3,4-Dichloropheny)-3-Methyl-Pyrazolone-5-one Synthesis

2012 ◽  
Vol 450-451 ◽  
pp. 223-227 ◽  
Author(s):  
Hui Qun Yu ◽  
You Bin Mo ◽  
Yan Fang Liao ◽  
Hai Zhou ◽  
Zhi Peng He
Keyword(s):  
Aqueous Medium ◽  
Ethyl Acetoacetate ◽  
Process Research ◽  
Raw Material ◽  
Reaction Condition ◽  
Phenylhydrazine Hydrochloride ◽  
New Process ◽  
Optimal Reaction Condition ◽  
Optimal Reaction ◽  
Chromatographic Purity

The new process of 1-(3,4-dichloropheny)-3-methyl-pyrazolone-5-one (34DCPMP) synthesis had been discovered, which using 3,4-dichloro phenylhydrazine hydrochloride(DCPH) and ethyl acetoacetate as the raw material , The product was obtained by the route during cyclization in aqueous medium. The structure of products was confirmed by 1HNMR, 13CNMR and IR. The effects of factors on the yield of products were investigated. It was found that the yield of 34DCPMP can reach 98.7% under the optimal reaction condition of n(34DCPH):n(ethyl acetoacetate) with 1:1.1, n(34DCPH):n(Na2SO3) with 1.3:1 at 80°C, and pH 7.5 for 3h. The chromatographic purity can be higher than 98.2%.

Two-Step Preparation of Bio-Diesel from the Used Bleaching Clay

2012 ◽  
Vol 209-211 ◽  
pp. 1774-1777
Author(s):  
Su Xi Wu ◽  
Shuai Hang Yan ◽  
Hui Cai
Keyword(s):  
Reaction Time ◽  
Maximum Yield ◽  
Acid Value ◽  
Raw Material ◽  
Bleaching Clay ◽  
Molar Ratio ◽  
Alkaline Catalyst ◽  
Orthogonal Experiments ◽  
Optimal Reaction Condition ◽  
Optimal Reaction

with the shortage of the raw material oil for producing bio-diesel in China, the oil, recovered from the used bleaching clay which often be discarded by vegetable oil factory, was used to prepare bio-diesel in this trial. Two-step catalyzed process was adopted to produce biodiesel from the oil. The effect of methanol-to-oil molar ratio, alkaline catalyst quantity, reaction temperature and reaction time on the preesterification and transesterification reaction was investigated through orthogonal experiments. Thus the optimal reaction condition came out. Firstly, the optimal pre-esterification condition, under which the end acid value of the product was minimum (i.e. 1.88 mgKOH/g),was to react for 40 h at 60°C,with a methanol-to-oil molar ratio of 12:1, and by adding alkali catalyst 4% based on the oil weight. Secondly，the optimal transesterification condition, under which the maximum yield of bio-diesel can reach up to 98.2%, was to react for 2.5 h at 60°C,with the methanol-to-oil molar ratio of 7:1, and by adding catalyst 1.25% based on the oil weight.

Improved Synthesis of 3,3-Dimethyl-4-Pentenoic Acid Methyl Ester

2012 ◽  
Vol 602-604 ◽  
pp. 1269-1273
Author(s):  
Yan Fang Liao ◽  
Hui Qun Yu ◽  
You Bin Mo ◽  
Hai Zhou ◽  
Chu He Peng
Keyword(s):  
Methyl Ester ◽  
Industrial Production ◽  
Recovery Rate ◽  
Sodium Methoxide ◽  
Acid Methyl Ester ◽  
Azeotropic Mixture ◽  
Acid Methyl ◽  
New Process ◽  
Optimal Reaction Condition ◽  
Optimal Reaction

The improved synthesis of 3, 3-dimethyl-4-pentenoic acid methyl ester (DPE) had been discovered. In new process, orthophosphate (85%) and sodium methoxide(98%)was used as catalysts at different stages of the reaction, the amount of azeotropic mixture of DPE and the byproduct 3'-methyl-2'-butenyl-3, 3-dimethyl-pentenpate (MBDP) is reduced, the recovery rate of product DPE is improved. under the optimal reaction condition, the highest yield of DPE approach 84%. Improved the process is more suitable for industrial production.

scholarly journals Optimization of reaction parameters for the green synthesis of zero valent iron nanoparticles using pine tree needles

2019 ◽  
Vol 8 (1) ◽  
pp. 846-855 ◽  
Author(s):  
Raziyeh Kheshtzar ◽  
Aydin Berenjian ◽  
Seyedeh-Masoumeh Taghizadeh ◽  
Younes Ghasemi ◽  
Ali Ghanbari Asad ◽  
...  
Keyword(s):  
Green Synthesis ◽  
Leaf Extract ◽  
Iron Nanoparticles ◽  
Zero Valent Iron ◽  
Effective Parameters ◽  
Reaction Condition ◽  
Pine Tree ◽  
Optimal Reaction Condition ◽  
Zero Valent Iron Nanoparticles ◽  
Optimal Reaction

Abstract In the current study, the optimal reaction condition for fabrication of INPs by using pine tree (Pinus eldarica) leaf extract was developed. A fractional factorial design was utilized to screen the effective parameters in the green synthesis reaction, and central composite face design was employed to achieve the optimal reaction condition. Leaf extract and iron precursor concentrations were found to be the most effective parameters for the fabrication of INPs. Physicochemical characteristics of the obtained nanoparticles were evaluated by transmission electron microscopy (TEM), Fourier transform infrared (FTIR) spectroscopy, X-ray diffractometer (XRD), vibrating sample magnetometer (VSM), thermogravimetric analysis (TGA), and derivative thermo gravimetric (DTG). The prepared particles were found to be zero-valent iron nanoparticles without any iron oxide impurities. Nanoparticles were spherical in shape with diameters ranging from 8 nm to 34 nm with a mean particle size of 18 nm. The fabricated particles were amorphous with a low magnetization value of 33 memu/g.

scholarly journals An Unexpected Reaction of Isodehydracetic Acid with Amines in the Presence of 1-Ethyl-3-(3-dimethylaminopropyl) Carbodiimide Hydrochloride Yields a New Type of β-Enaminones

Molecules ◽  
2020 ◽  
Vol 25 (9) ◽  
pp. 2131
Author(s):  
Delong Wang ◽  
Hui Shi
Keyword(s):  
Coupling Agent ◽  
Simple Method ◽  
Reaction Condition ◽  
Carbodiimide Hydrochloride ◽  
Unexpected Reaction ◽  
Optimal Reaction Condition ◽  
New Type ◽  
Optimal Reaction

The reaction of isodehydracetic acid with amines was serendipitously found to afford β-enaminones in the presence of the coupling agent 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide hydrochloride (EDC). Under the optimal reaction condition, 23 examples of α-aminomethylene glutaconic anhydride were obtained at approximately 30−80% yields. This is a concise, operationally simple method to expediently synthesize a new type of β-enaminone-containing compound.

Enzymatic saccharification of cellulose in aqueous-ionic liquid 1-ethyl-3-methylimidazolium dimethylphosphate-DMSO media

2011 ◽  
Vol 65 (6) ◽  
Author(s):  
Yu He ◽  
Cui Ma ◽  
Dong Xia ◽  
Liang Ding ◽  
Liang Li ◽  
...  
Keyword(s):  
Saccharomyces Cerevisiae ◽  
Ionic Liquid ◽  
Ethanol Production ◽  
Enzymatic Saccharification ◽  
Environment Friendly ◽  
Reaction Condition ◽  
Optimal Reaction Condition ◽  
Optimal Reaction ◽  
Cellulose Materials

AbstractIonic liquid (IL) 1-ethyl-3-methylimidazolium dimethylphosphate ([Emim]DMP) was chosen as an environment-friendly solvent to enzymatically hydrolyze cellulose in situ. Under optimal reaction condition, 80.2 % of cellulose (10 mg mL−1) were converted to glucose in aqueous-IL-DMSO (φ r = 74: 25: 1) media at 55°C in 18 h. Finally, fermentability of the recovered hydrolyzates was evaluated using Saccharomyces cerevisiae which is able to ferment hydrolyzates efficiently, the ethanol production was 0.44 g g−1 of glucose within 24 h of the process. Such information is vital for the saccharification of more complex cellulose materials and for the fermentation of hydrolyzates into biofuel.

scholarly journals Chitinase GenesLbCHI31andLbCHI32fromLimonium bicolorWere Successfully Expressed inEscherichia coliand Exhibit Recombinant Chitinase Activities

2013 ◽  
Vol 2013 ◽  
pp. 1-9 ◽  
Author(s):  
Zhihua Liu ◽  
Ying Huang ◽  
Rongshu Zhang ◽  
Guiping Diao ◽  
Haijuan Fan ◽  
...  
Keyword(s):  
Cell Wall ◽  
Optimal Condition ◽  
Cell Walls ◽  
Recombinant Enzymes ◽  
Extracellular Medium ◽  
Fungal Cell ◽  
Reaction Condition ◽  
Recombinant Chitinase ◽  
Optimal Reaction Condition ◽  
Optimal Reaction

The two chitinase genes,LbCHI31andLbCHI32fromLimonium bicolor, were, respectively, expressed inEscherichia coliBL21 strain. The intracellular recombinant chitinases, inrCHI31 and inrCHI32, and the extracellular exrCHI31 and exrCHI32 could be produced intoE. coli. The exrCHI31 and exrCHI32 can be secreted into extracellular medium. The optimal reaction condition for inrCHI31 was 5 mmol/L of Mn2+at 40°C and pH 5.0 with an activity of 0.772 U usingAlternaria alternatacell wall as substrate. The optimal condition of inrCHI32 was 5 mmol/L of Ba2+at 45°C and pH 5.0 with an activity of 0.792 U usingValsa sordidacell wall as substrate. The optimal reaction condition of exrCHI31 was 5 mmol/L of Zn2+at 40°C and pH 5.0, and the activity was 0.921 U using theA. alternatacell wall as substrate. Simultaneously, the optimal condition of exrCHI32 was 5 mmol/L of K+at 45°C and pH 5.0, withV. sordidacell wall as the substrate, and the activity was 0.897 U. Furthermore, the activities of extracellular recombinant enzymes on fungal cell walls and compounds were generally higher than those of the intracellular recombinant enzymes. Recombinant exrCHI31 and exrCHI32 have better hydrolytic ability on cell walls of different fungi than synthetic chitins and obviously showed activity againstA. alternata.

Direct Synthesis of 3,5-Dinitropyrazole Catalyzed by Newly Sulfated Nanosolid Superacid TiO2/ SO

2011 ◽  
Vol 391-392 ◽  
pp. 1296-1301
Author(s):  
Li Min Xi ◽  
Xin Xin Zhang
Keyword(s):  
Direct Synthesis ◽  
Sol Gel ◽  
Acid Base ◽  
Direct Transformation ◽  
Acid Base Titration ◽  
Optimal Reaction Condition ◽  
Superacid Catalyst ◽  
Average Size ◽  
Optimal Reaction ◽  
Xrd And Tem

The newly sulfated nanosolid superacid TiO2/SO4 prepared by sol-gel method was broadly characterized by acid base titration, XRD and TEM, which identified that the superfine solid TiO2/SO4 showing good dispersibility with average size of 27 nm belongs to kind of crystalline nanoparticles. With the help of the catalyst TiO2/SO4, the optimal reaction condition for direct transformation of pyrazole and nitrosonitric acid into 3, 5-Dinitropyrazole was n (pyrazol)=0.10 mol, m (TiO2/SO4 )＝1.5g, V(n-octannol)＝90mL, and V(nitrosonitric acid)＝50mL. Moreover, the optimal yield of the catalytic reaction reached up to 59.4% when the reaction time is 7 hours. The nanosolid superacid catalyst is still of high activity after regenerating eight times by calcination at 600。C.

Production of Primary Magnesium by the Aluminothermic Reduction of Magnesia Extracted from Dolomite Ore

2014 ◽  
Vol 788 ◽  
pp. 28-33
Author(s):  
Peng Deng ◽  
Yu Qin Liu ◽  
Wen Gui Yao ◽  
Hong Wen Ma
Keyword(s):  
Calcium Carbonate ◽  
Magnesium Oxide ◽  
Vacuum Condition ◽  
Reduction Ratio ◽  
Raw Material ◽  
Aluminothermic Reduction ◽  
Molar Ratio ◽  
New Process

In this paper, a new process for the production of the primary magnesium is introduced using the dolomite as the raw material. The magnesia and calcium carbonate were prepared from dolomite by acidification. The content of magnesium oxide can reach 98.92% about the magnesia obtained. The magnesia is used to produce primary magnesium by aluminothermic reduction under vacuum condition. The reduction ratio of MgO can be up to 86.14% under the temperature of 1200°C for 5hrs, briquetting pressure of 10MPa and the molar ratio of MgO to Al of 3:2. The content of magnesium is more than 99.90%. The major phases in the briquette residue are corundum and spinel, which can be used as refractory.

Hydrothermal Synthesis of GdVO4:Eu 3+ Phosphors by Optimizing its Preparation Conditions

2011 ◽  
Vol 287-290 ◽  
pp. 1360-1364
Author(s):  
Ying Lin Yan ◽  
Yun Hua Xu ◽  
Juan Wang ◽  
Zhen Xing Luan
Keyword(s):  
Ph Value ◽  
Photo Luminescence ◽  
Luminescence Spectroscopy ◽  
Temperature Reaction ◽  
Hydrothermal Temperature ◽  
Red Emission ◽  
X Ray ◽  
Preparation Conditions ◽  
Optimal Reaction Condition ◽  
Optimal Reaction

Eu3+ -doped GdVO4 powders have been synthesized via a novel hydrothermal method using commercially available Gd2O3, NH4VO3 and Eu2O3 as the reacting precursors. The influences of several important parameters, such as hydrothermal temperature, reaction time and pH value, of the experiment were investigated. The obtained samples were characterized by X-ray powder diffraction (XRD), field emission scanning electron microscopy (FESEM), and photo-luminescence spectroscopy (PL). The experimental results showed that the optimal reaction condition was processed at 180°C for 12 h and adjusted pH value to 4. The morphology of products was uniform pseudo-octahedron with a little conglomeration. All the phosphors exhibit the characteristic dominant red emission of Eu3+ ion (5D0 → 7F2) at 618nm.

Sign in / Sign up

Export Citation Format

Share Document