2013, 30(11).
Abstract:The viscosity behaviors of polyacrylamide fracturing fluid had been studiede through investigating the concentration,temperature,pH and metallic ion .The results showed that,when increased the PAM concentration, the fracturing fluid viscosity increased, non-Newtonian viscosity enhanced and the viscosity of fracturing fluid could meet the construction requirements when the concentration was 1.0%. increased the temperature could decrease the fracturing fluid viscosity and weaken non-Newtonian. Change the PAM fracturing fluid pH environment also could decrease the viscosity. Metal ions could decrease the viscosity of fracturing fluid, the effect of metal ions on PAM viscosity order was Mg2+>Ca2+>Na+>K+, consisted with diffusion layer theory. The static suspension experiments showed that when the PAM concentration of 1% and 60 ℃,,the proppant-carrying time reached 16.58min/cm,,could meet the fracturing fluid carrying sand standards.
2013, 30(11).
Abstract:Using 1-bromo-3-fluorobenzene、4-bromobenzonitrile、1-(trans-4-propylcyclohexyl)-1-chloro-methane etc as starting materials, 2,6 - difluoro-4 - [3 - fluoro-4'-[1 - methyl - 2 - (4 -propylcyclohexyl) - ethyl]-biphenyl]phenyl difluoromethoxy-3, 4,5 - trifluorobenzene was synthesized by a method consisting of seven steps: Grignard reaction、Suzuki reaction、Witting reaction、hydrogenation reaction, etc. The reaction solvent of grignard reagent and 4-bromobenzonitrile was xylene;the optimum reaction time of lithiation reaction was 2h . The overall yield was about 30% and the purity reached 99.7%(GC)(mp:82.97-85.04℃). Adding the compound into base composition of liquid crystal can improve the birefringence (Δ n),reduce the threshold voltage(Vth).
QI Xiu-fang , WANG Ming , WEI Li-cheng , CHENG Guang-bin , LU Chun-xu
2013, 30(11).
Abstract:With fuming nitric acid (95%) as the nitrating agent, six water magnesium nitrate as assistant, process improvement exploration was carried out for the synthesis of high energy explosive hexogen (RDX) by direct nitrolysis of urotropine. Based on the direct method, three main factors on the yield of RDX were investigated, such as the effects of the amount of Mg(NO3)2?6H2O, reaction temperature and reaction time in maturation period. The optimum synthesis conditions were obtained, which are: molar ratio of Mg(NO3)2 ?6H2O to HA: 1︰2; the temperature of maturation period: 30 oC; the reaction time in maturation period: 60min. The optimized process can improve the yield of RDX to 80.6%, 8.6% higher than the original process.
Lu Hong-sheng , Yuan Xiao , Huang Zhi-yu
2013, 30(11).
Abstract:Quadripolymer AMPF was synthesized with sulfanilic acid(C6H7NO3S), p-methyl benzenesulfonic acid(C7H8O3S), phenol(C6H6O) and formaldehyde(CH2O). By taking the single factor analysis method , the optimal pH synthesis condition of product is 9;molar ratio of monomer n(C6H7NO3S):n(C7H8O3S):n(C6H6O):n(CH2O)is 1:4:6:13.2; the reaction temperature is 75 ℃. Meanwhile, the structure of this reducer is clarified though infra-red spectrum, 1H—NMR spectrum and the results show that the molecular structure of artificial synthesis product is in accord with ideal one. The thermogravimetric experiment indicates good thermal stability of this reducer. Moreover, this polymer has been demonstrated with good temperature resistance, salt tolerance and excellent compatibility.
2013, 30(11).
Abstract:The comb polysiloxane crude oil demulsifier that the main chain was silicone oil and had multi-branched chain was synthesized by the hydrosilylation reaction with the allyl polyether acrylate, methyl acrylate, methyl methacrylate,using isopropanol as the solventand, chloroplatinic acid as the catalyst and at the reaction temperature of 95℃. The author determined the optimum ratio of 3:2:2 by investigating the effects on the dehydration efficiency of the Yan'an crude under different ratios of the allyl polyether ester, methacrylic acid, methyl methacrylate and study the function of comb crude oil demulsifier on the Yan'an crude oil through the the demulsification performance test. In addition, blending the product with TA-1031 in proportion 3:2 at the total plus the amount of 100mg?L-1, at the dehydration temperature of 60℃, made the dehydration rate achieve 91.02%.
2013, 30(11).
Abstract:2-(2-Hydroxyphenyl)cyclopropane-1-carboxlic acid (HCCA) was prepared from the starting material of 2-methoxystyrene via the chlorine-addition, cyclopropanation reaction with diethyl malonate, Krapcho decarboxylation and demethylation using thiophenol as nucleophiles under alkali conditions with a high total yield of 53%. The target product was also confirmed through 1H NMR, 13C NMR, GC-MS and HRMS. The synthetic process of HCCA can be performed under mild reaction conditions with conveniently available reagents and good yields, providing a potential route for the large-scaled syntheses.
2013, 30(11).
Abstract:Chloride 1-benzyl-3-(3,5-bis (trifluoromethyl)) phenyl imidazole salt and bromide 1- decyl-3-(3,5-bis (trifluoromethyl)) phenyl imidazole salt were synthesized from 3,5-bis (trifluoromethyl) aniline, formaldehyde, glyoxal, ammonium chloride and benzyl chloride or 1-bromodecane by condensation reaction, nucleophilic substitution reaction and the yields were 59.0% and 77.1%. The compounds of 1-benzyl-3-(3,5-bis (trifluoromethyl)) phenyl imidazole tetrafluoroborate and 1-benzyl-3-(3,5-bis (trifluoromethyl)) phenyl imidazole hexafluorophosphate were designed and synthesized by anion exchange reaction of chloride 1-benzyl-3-(3,5-bis ( trifluoromethyl)) phenyl imidazole salt. All the compounds were characterized by means of 1H NMR and 13C NMR. The effect of solvent on the nucleophilic substitution reaction was studied. The results demonstrated that toluene as solvent, the yield was 59.0%.
WANG Liu-cheng , JIN Lin-feng , ZHAO Jian-hong , WANG Jian-she , CHENG Xiang-lin , SONG Cheng-ying
2013, 30(11).
Abstract:Using methyldichlorosilane with 1-dodecene as materials have successfully synthesized dodecylmethyldimethoxysilane using self-made platinum catalyst, and then dodecylmethyldimethoxysilane was synthesised via alcoholysis reaction through atmospheric liquid-phase reaction. The structure of target compound was characterized by means of 1HNMR and IR spectrum. The reaction conditions have been optimized as follows: feeding speed of dodecene 5mL/min, n(methyldichlorosilane)∶n(1-dodecene)=1.1∶1, m(platinum catalyst)∶m(methyldichlorosilane) = 1.5×10﹣4∶1, reaction temperature 110℃, reaction time 20min and the yield of intermediate product could reached 92.5%, selectivity to β-addition product was 100%. Feeding speed of intermediate product 1mL/min, methanol steam flow 1500mL/min, eaction temperature 85℃, the purity of the dodecylmethyldimethoxysilane was 97% after the separation and purification processes,the yield of product could reached 90.5% .
XIA Ru , Bu Yi , Chen Peng , Qian JIa-sheng , Miao Ji-bin , Yang Bin , Su Li-fen
2013, 30(11).
Abstract:Macroinitiator (PAN-Br) and block copolymer (PAN-b-PZDMA) are synthesized using Atom Transfer Radical Polymerization (ATRP). The viscosity-average molecular weights of PAN-b-PZDMA we prepared are 7507,8517,9905 respectively. The molecular structures of macroinitiator and block copolymer (PAN-b-PZDMA) are characterized by 1H-NMR and FT-IR. It was shown by TGA and DSC that the thermal stability of block copolymer is promoted by the block of PZDMA in copolymer.
PANG Jian-jun , WANG Dong-min , WANG Dong , SUN Yun-ming , ZHANG Li-ran
2013, 30(11).
Abstract:Multiple pharmacological activities were influenced of its activity of scavenging free radicals. The activity that different substituted theanine analogs at 5 position scavenge free radicals was studied in order to find the lead compound whose ability of scavenging free radicals was excellent. 7 kinds of analogs of theanine were synthesized via protection of phthalic anhydride, acylation and opening ring, deprotection of hydrazine hydrate from L-glutamic acid in the paper. The structures of the synthesized compounds was confirmed by IR,1H NMR and 13C NMR, and their activity of scavenging DPPH free radical and hydroxyl free radical were determined as well. The results indicated that the activity of scavenging free radical of 2-amino-5-((4-hydroxyphenyl)amino)-5-oxopentanoic acid was the best of the seven chemicals, whose rate of scavenging DPPH free radical was 90% at 0.002 mol?L-1 and rate of scavenging hydroxyl free radical was 95% at 0.004 mol?L-1. Followed was 2-amino-5-((4-aminophenyl)amino)-5-oxopentanoic acid. These showed that it could enhance the theanine ability of scavenging DPPH free radical and hydroxyl free radical that its 5 position was substituted by phenyl linking with nothing or electron donating group at 4 position. And the electron donating ability of group was stronger, the activity of scavenging free radicals was better.
2013, 30(11).
Abstract:Abstract:More than 95% purity of fine chemical intermediates of 1-(4-bromo-phenyl)-propenone was synthesized via Friedel-Crafts and elimination reaction with bromobenzene as the starting material. The target compound was characterized by 1HNMR、IR and GC-MS. The best reaction conditions of Friedel-Crafts and elimination reaction were investigated. The results of condition experiments showed that when n(3-chloropropionyl chloride):n(bromobenzene):n(aluminium chloride)=1.3:1:1.5, and the reaction temperature was 20~25 ℃, the reaction effect of Friedel-Crafts was best. With potassium acetate as the base, when n[1-(4-bromo-phenyl)-3-chloro-propan-1-one]: n[potassium acetate]=1:1.5, and the reaction temperature was 20~25 ℃, the reaction effect of elimination reaction was best.
2013, 30(11).
Abstract:In this paper, PAM was synthesized by photoinitiated polymerization. The methods of orthogonal design and uniform design were employed to optimize polymerization conditions, and the experimental data were manipulated by the mathematical analysis software SPSS. The effects of light intensity, the inner diameter of reaction vessel, rotation speed and reaction time for the polymer solution viscosity were explored. The results showed that the optimum polymerization conditions were described as follows: light intensity was 0.15 mW/cm2, the inner diameter of reaction vessel was about 36 mm, rotation speed was 10 r/min, and polyreaction 2 h. Finally we obtained that the relative molecular weight of PAM was more than 20 million.
2013, 30(11).
Abstract:Super absorbent polymer (SAP) was synthesized by aqueous solution polymerization. Then SAP was post-processed with a mixture of aluminum sulfate, glycerol and ethylene glycol diglycidyl ether. The influences of the amount of different surface crosslinking agents, surface crosslinking temperature and dosage of surface crosslinking solution on the performance of SAP were investigated. SAP was also characterized by FIIR and SEM. The results showed that, the absorbency capacities increased with the rising amount of aluminum sulfate while AUL decreased. Oppositely, the absorbency capacities decreased with the increasing dosage of ethylene glycol diglycidyl ether and surface crosslinking temperature while AUL increased. The maximum absorbency capacities for deionized water and saline water were 685g/g and 79g/g respectively when the mass fraction of glycerol was 9%, and AUL reached its maximum when the mass fraction of glycerol got to 12.7%. When the amount of surface crosslinking solution was 7.7g, the combination properties of SAP were the best.
SHA Xue-fei , CHEN Lihua , DU Yang , jiangdi
2013, 30(11).
Abstract:The 1,2,3,5-tetra-O-benzoyl-2-C-methyl-βD-ribonfuranose was synthesized from D-fructose by four steps, which were lactonization, acylation, reduction, and acylation, the overall yield was 10.6%. The characterization methods of 1HNMR、13C-NMR and MS were applied to confirm the structures of intermediates and product. Combining with the reduction condition, the best raw material for synthesizing 2-C-Methyl-D-ribonic-γ-lactone were D-fructose and CaO. The conclusion that the best reductant for 2,3,5-Tri-O-benzoyl-2-C-methyl-βD-ribofuranose is Red-Al was obtained by comparing using three different reductant as LiAlH4, NaBH4 and Red-Al and the yield can up to 96.20%.Through single factor experiments determented that triethylamine was the best acid binding agent for acylation reaction and the yield can up to 75.84%.
2013, 30(11).
Abstract:In this paper, sebaconirile had been successfully prepared using sebacic and ammonia as raw materials under the condition of catalysts. The effects of catalysts with different compositions, reaction temperature and time were studied. The results showed that the optimal synthesis condition as follows: the lower temperature region (140-210 oC) were favorable for amidition reaction and the corresponding reaction time is 8h, however the dehydration reaction is very effective under the higher temperature region (210-265 oC) and the corresponding dehydration time is 5h. ZnO/Al2O3 catalysis with mass faction of 6% revealed the yield of 83%. The crude product had been characterized by HNMR and the purity of prepared sebaconitrile was 92% via temperament chromatograph , which indicated that the sebaconitrile synthesized in this paper would have the good value of industrialization
2013, 30(11).
Abstract:1,4-butanediol Gemini Sodium lauryl polyoxyethene(3) iso-octyl sulfosuccinate was synthesized under normal pressure by using carbon-based solid acid as the catalyst in esterification,an environmentally friendly process where purification and separation of the intermediates and organic solvents in reaction esterification is unnecessary. The optimum reaction conditions were as follows: For the single esterification , n (maleic anhydride) : n (1, 4 - butanediol) = 2.15:1.00, and reacted at 110℃ for 2.0h with the yield of 99.23%.For the diesterificationⅠ: n (maleic anhydride) : n (lauryl polyoxyethene(3)) = 1.00:0.55, ω (carbonyl solid acid) = 1%(with the quality of maleic anhydride calculated), and reacted at 170℃ for 2.0h. For the diesterification Ⅱ: n (maleic anhydride) : n (iso-octanol) = 1.00:0.60, and reacted at 220℃ for 4.5h with the yield of 94.36%. For the sulfonation reaction: n (maleic anhydride) : n (sodium hydrogen sulfite) = 1.00:1.05, and reacted at 140℃ for 5.5h with the target product. The structure of product was characterized by IR spectrum and GC/MS, the surface properties and application properties were measured, and it was compared with sodium lauryl polyoxyethene(3) isoctyl sulfosuccinate (AEOSS3) and 1, 4 - butanediol Gemini sodium diisooctyl sulfosuccinate(GSS462).The results showed that the critical micelle concentration of GSS4AEO3-62 reduced one to two orders of magnitude than AEOSS3 and GSS462 and the toxicity were also low.
2013, 30(11).
Abstract:3%MoO3/γ-Al2O3 catalysts with different Re2O7 contents were prepared via conventional incipient-wetness impregnation method. Mixed butene self-metathesis reactions over these catalysts were investigated in a fixed-bed reactor, where mixed butene (n(1-butene)∶n(2-butene)=3) was chosen as reactant. The catalysts were characterized by means of XRD,NH3-TPD,H2-TPR and N2-adsorption. The results indicate that addition of rhenium in 3%MoO3/γ-Al2O3 catalyst increased the acid amount, inhibited the induction period in the initial stage of the reaction, enhanced the activity and stability of catalysts in mixed butene self-metathesis reaction. Under the reaction conditions of 80 ℃, 1.0 MPa, WHSV=1.2 h-1, 1%Re2O7-3%MoO3/γ-Al2O3 catalyst gave butene conversion above 60%, propene yield remained at about 25% during 70 h on stream.
LI Ying-jiao , TAO Bo , LIU Yu-chen
2013, 30(11).
Abstract:At first, 4-nitro-3-hexanol, 3-nitro-4-heptanol and 2-nitro -1-phenyl -1-propanol were synthesized with nitroalkane and aldehyde ; then they were reduced to 4- amino -3-hexanol, 3 amino -4-heptanol and 2- amino -1-phenyl -1-propanol with iron powder and concentrated HCl . The six title compounds as latent herbicide safener were prepared from amino alcohol, acetone and dichloroacetyl chloride with triethylamine as acid acceptor in the yield of 54.58%、74.39%、53%、79%、88.52% and 66.72%。 respectively. The structures of the compounds were confirmed by IR、 1H NMR、13C NMR and elemental analysis,and the compound of Ⅲc was further characterized by X-ray diffraction. The preliminary biological test show that the recovery rates of the plant height could attain 81.92% with 50μM of compound Ⅲc when the concentration of acetochlor in the soil was 10mg/kg.
MA Li , DAI Ya-tang , OU Qing-hai , WANG Wei , ZHANG Huan , Chen Yu-hua
2013, 30(11).
Abstract:Doped Ti4 -LiFePO4/C was synthesized by a step hydrothermal method at different temperatures using (NH4)2FeSO4、LiOH、Ti(SO4)2 and H3PO4 as raw material and then modified with carbon coating. X-ray diffraction patterns and scanning microscopy images along with energy dispersive spectroscopy mappings have verified the com electron homogeneous existence of coated carbon and doped Ti4 in LiFePO4 particles with phospho-olivine structure and an average size of 140 nm at 160℃. The electrochemical performances of the material have been studied galvanostatic charge-discharge measurements and electrochemical impedance spectroscopy. The results show the material is the best electrochemical performance at 160℃. The initials discharge capacity of 160.97mAh g?1 at 0.1C, a capacity retention of 95.28% after 50 cycles at 0.5C and a increased lithium ion diffusion coefficient of 1.78?0-12 cm2 s-1.
2013, 30(11).
Abstract:1-ammonia propyl-2-methyl imidazole was synthetizatied from catalytic hydrogenation of 1-cyanoacetate-2-methylimidazole (2MZCN), the parameters of synthetic process were investigated systematicly .And the appropriate synthetic conditions were obtained. The conversion of 2MZCN and 1-amino-propyl-2-methyl imidazole yield reached 99.7% and 94.2% after reaction 4 h respectively, under the conditions of reaction temperature of 100℃, pressure of 5Mpa, speed of 624rpm, and the solvent is saturated ethanol solution of ammonia (ratio with the quality of raw material is 2:1), Rainie nickel is the catalytic agent and potassium hydroxide act as catalyst promoter (accounting for the quality of raw material 18.9%). The product is analysed by Infrared spectroscopy (FTIR) and proton nuclear magnetic resonance spectroscopy (1H-NMR) and Gas Chromatography-Mass Spectrometer(GC-MS).
2013, 30(11).
Abstract:A novel type of cationic-nonionic gemini surfactant DAEQ9-Cl was synthesized with lauryl alcohol polyoxyethylene (9), dimethyl sulfoxide and tetramethylethylenediamine as the main starting materials. The main reaction includes chlorination and quaterisation. The optimum reaction conditions was ascertained as follows: n(dimethyl sulfoxide) : n(lauryl alcohol polyoxyethylene (9)) = 1.5 : 1, the reaction taking place at 80 oC for 8h, with pyridine as catalyst, the yield was 87%. In the quaterisation process, intermediate and tetramethylethylenediamine (2:1) reacted at 80 oC for 3d, the yield was 79%. The target product was identified by IR and 1H NMR. The critical micelle concentraton (cmc) is 3.2×10-2 mmol/L and γcmc is 33.44 mN/m at 25 oC in aqueous solution. DAEQ9-Cl shows a synergic effect when blended with AEO-9. The best compatibility effect was achieved at a molar of 4 : 6. The best compound system shows cmc=6.78×10-3 mmol/L, γcmc=28.5mN/m. This new surfactant exhibits higher foaming ability and foam stability.
XIONG Li-zhi , LI Zi-wei , OUYANG Wen , ZHANG Xiao-rong , LI Gui , LI Na
2013, 30(11).
Abstract:Flavonoids were extracted under ultrasonic assistance from Artemisia Annua L. residue where Artemisinin was extracted, using ethanol as extraction solvent. The optimal ultrasonic-assisted extraction technology was determined by single factor experiment and orthogonalexperiment. Meanwhile,antioxidant activity of flavonoids which were purified to oil and fat was evaluated and compared with that of ascorbic acid and citric acid. Results showed: the optimal ultrasonic-assisted extraction technology of flavonoids in Artemisia Annua L. residue is: ethanol volume fraction about 50% , material-to-liquid ratio of 1∶30 (g:mL), ultrasonic power of 200 W , ultrasonic-assisted extracting time about 40 min and extraction temperature at 55℃. The extraction rate of flavonoids reaches 9.10% with the optimal ultrasonic-assisted extraction technology. The removal efficiency of hydroxyl radical increases along with the increase of the purified flavonoids concentration. The purified flavonoids reveales obvious antioxidant effect on oil and fat, it is superior to not only ascorbic acid but also citric acid on oil , it is somewhat higher than that of citric acid but inferior to ascorbic acid on fat.
JI Hong-bing , ZHAO Mingyue , FANG Yanxiong , YANG Zhujin , YIN Xueqiong
2013, 30(11).
Abstract:Chitooligosaccharide/salicylic acid microcapsules have been prepared by spray-drying method and the preparation conditions were optimized using the single factor study with oil content and encapsulation efficiency of the microcapsules as criteria. The optimal production conditions are as follows: ρ(chitooligosaccharide)= 2%(w/w), m (chitooligosaccharide):m (salicylic acid) = 1.0:0.5, inlet temperature =170癈, drying air speed= 3.9 m?s-1, rotational speed of pump feed = 8 RPM. Oil content and encapsulation efficiency of the product were 19.1% and 21.5%, respectively. The encapsulation has been confirmed by observing the morphology of microcapsules. The particle size analysis suggested that the average particle size of microcapsules was in the range of 3.154μm ~ 19.751μm. FTIR spectra were used to prove the existence of intermolecular interaction between salicylic acid and chitooligosaccharide. TG-DSC results confirmed the thermal stability of salicylic acid was improved after encapsulating by chitooligosaccharide.
KE Yong , SHEN Yi-ding , FEI Gui-qiang , WANG Hai-hua
2013, 30(11).
Abstract:Abstract:Modified polyvinyl alcohol (PVA) fibers with reaction activity were synthesized via suspension grafting copolymerization using glycidyl methacrylate (GMA) as functional monomer. The effects of modified PVA fiber mass fraction and drying temperature on folding endurance, tensile strength and wet strength were investigated. The results show that the desired condition for a better strength of paper is as follow: the mass fraction of modified PVA fiber is 9%, drying temperature is 110℃. At this time, folding endurance is 73 times, dry tensile strength is 70.4N, wet tensile strength is 16.2N. The structure of modified PVA fibers was characterized by TGA, which showed that the grafting copolymerization of GMA took place on the surface of PVA fiber. AFM photographs show that the formation of mastoid structure on the surface of modified PVA fiber contributes to the creation of hydrophobic surface. SEM photographs show that the length of fibers on the fractured edge of paper containing modified PVA fibers is shorter and the dissolution degree of modified PVA fibers is decreased significantly.
ZHOU Shou-fa , LIU Ai-ying , PANG Hao , JI Hong-guo , LIAO Bing
2013, 30(11).
Abstract:Poly (acrylic acid-co-Allyl glycidyl ether) for ceramic dispersantion was synthesized. Ammonium persulfate was used as initiator agent, and the sodium hypophosphite was a chain transfer agent for synthesis. The reaction was monitored by online infrared, and the molecular weight was measured by gel-permeation Chromatography (GPC). The effects of synthesis conditions, such as concentration of acrylic acid, ammonium persulfate, sodium hypophosphite reaction temperature and reaction time were investigated respectively. The effect of dispersant weight on Zeta potential value and suspension rhelogy behavior were measured as well. The online IR showed that polymer was poly (acrylic acid co-maleic anhydride) sodium, its optimal synthetic conditions were got as follows: w(acrylic acid) 28wt%, ammonium persulfate 0.17 g, sodium hypophosphite 2 g, allyl glycidyl ether 0.9mL, reaction temperature 80 ℃, reaction time 3.5h. The lowest Zeta potential value was -66.7mV, when dispersant weight concentration was 150mg/L, the shear stress reduced along with the increased dispersant weight.
ZHANG Fei , WANG Shirong , LI Xiang-gao , GUO Jun-jie
2013, 30(11).
Abstract:7-hydroxy-4-methylcoumarin was synthesized by resorcinol and ethyl acetoacetate under the catalysis of concentrated sulfuric acid. Then 4-nitro-phthalimide as raw materials was first in the open-loop catalytic ammonia and then by the dehydration with phosphorus oxychloride to get 4-nitro-phthalonitrile. The two obtained compounds by nucleophilic substitution reaction were reacted to form 7-(3,4-dicyanophenoxy)-4-methylcoumarin. By investigating the feed ratio, the amount of acid binding agent, the reaction temperature and reaction time, we confirmed the optimal reaction conditions which were 7-hydroxy-4-methylcoumarin,4-nitro-phthalonitrile and anhydrous potassium carbonate whose molar ratio were 1.4:1.0:1.5 , the temperature 30 ℃, reaction time 14 h and the yield 63.7%. And the structures of compounds synthesized have been confirmed by IR, 1H-NMR and high performance liquid chromatography(purity 99.30 %).By enlarging the experimental conditions, we get the yield about 83.1% which is higher than the reported yield 68%.
SONG Guo-qiang , WANG Rui-rui , LI Bei-bei , FENG Xiao-qing
2013, 30(11).
Abstract:1, 5 - diaza-bicyclo [4.3.0]-5-nonene (DBN), which usually plays an important role as a catalyts in organic synthesis due to its strongly basic, is developed in the 1960s. In this paper, 1, 5-diazabicyclo[4,3,0]nonane was prepared by reduction of 1,5-diazabicyclo[4,3,0]nonene(DBN) with LiAlH4 in methyl tert-butyl ether at 55℃ for 9h. The yield and purity of the product can reach 87.9% and 95%, respectively. This series of amidine photobase generators was synthesized through the reaction of 1, 5-diazabicyclo[4,3,0]nonane with corresponding chloro-methyl-pyridine compounds and the yield and purity was even up to 84.7% and 95.7%, respectively. The structure-activity relationship of the photobase- generators was investigated by UV absorbance, thermal stability and photo-sensitivity and so on. HPLC, LC-MS and 1H-NMR were also applied to monitor and characterize the intermediates and products.