Yield 67%. In a 50 mL two neck round-bottomed flask was weighed N1,N2-bis[2,6-bis(1-methylethyl)phenyl]-1,2-benzenediamine (7, 100 mg, 0.23 mmol) and triethyl orthoformate (20 mL) was added and a fractional distillation apparatus equipped with a Vigreux column and a thermometer on the head of the latter was connected with the central neck of the flask. Keywords: benzimidazolium salts; bulky ligands; cyclization; ligand design; N-heterocyclic carbenes (NHC); ring formation. G. Andrew Woolley, © 2015 Grieco et al; licensee Beilstein-Institut. Fang, W.; Jiang, J.; Xu, Y.; Zhou, J.; Tu, T. Gürbüz, N.; Yaşar, S.; Özcan, E. Ö.; Özdemir, I.; Çetinkaya, B. Türkmen, H.; Pape, T.; Hahn, F. E.; Çetinkaya, B. Methyl alcohol (or ethanol) and sodium hydroxide, haloform reaction separate salt, and the fractionation by distillation product according to synthetic liquid gas chromatographic analysis, is that benchmark calculates with sodium hydroxide, and yield is 61.2%, reacts 12 hours. We expected high yields and reduced overall reaction times when compared with the previously reported synthetic pathways. Proportioning raw materials ginseng is shown in Table 2: The dehydrating effect comparison of dewatering agent of the present invention: Group: be divided into four groups, wherein, control group 1: do not add any dewatering agent; Control group 2: glycerol; Control group 3: glycerol+4A molecular sieve (mass ratio is 5: 1); The present invention: glycerol+atlapulgite+4A molecular sieve (mass ratio is 5: 1: 1).The addition of above-mentioned dewatering agent is 2% of solvent quality.Detect moisture and triethyl orthoformate product yield in the mixed solution after alcoholysis, specifically referring to table 3: Group Sterically demanding benzannulated NHCs bearing mesityl rings. Be understandable that, the present invention can also make other restriction, and other of making on the basis of the embodiment of the present invention improve still within protection scope of the present invention. ), HCOOH, 80 °C [44]. All manipulations were carried out under an atmosphere of dry nitrogen using standard Schlenk techniques or in a glove box (M. Braun 150B-G-II) filled with dry nitrogen. Triethyl orthoformate synthetic method simple possible of the present invention, is applicable to large-scale industry and changes into product. To avoid this complication 1,2-dibromobenzene had to be applied to eventually approach the preparation of 7. Proportioning raw materials ginseng is shown in Table 1: First in and crystallization kettle add 60% solvent, be cooled to 0 ℃ of left and right, add ethanol, while continuing to be cooled to subzero 5 ℃, add dewatering agent, the addition of dewatering agent is 2% of solvent quality, then pass into HCl gas, continue to be cooled to subzero 7 ℃ of left and right, add imines, then slowly add other 40% solvent, in after 1 hour, finish with crystallization, be discharged to alcoholysis still, be warming up to 20 ℃ of left and right, add alcoholysis ethanol, after insulation reaction 10 hours, carry out centrifugation and obtain mixed solution, through distillation, can obtain finished product triethyl orthoformate again, the solid that centrifugation obtains is ammonium chloride, as byproduct, sell outward. Alternatively, since peptides with N-terminal Gln residues undergo spontaneous cyclization to pyro-Glu, this mechanism may be sufficient to maintain normal function. Then concentrate, can to obtain purity be triethyl orthoformate 98% or more in rectifying, recyclable solvent of washing water and salt, the mixed solvent that reclaims in the concentrated rectifying can be used as entrainer to be continued to recycle. [47]. Figure 1: III. 276700 Linshu County, Shandong City, Linyi province Linshu County Huasheng Chemical Co., Ltd. Linshu County Huasheng Chemical Co., Ltd. 301, room 1, unit 29, building 276700, building 19, Cang Ma Xi Street, Linshu, Shandong, 原甲酸三乙酯合成液中微量水分的脱除, The synthesis technique of trimethyl orthoformate, Process for the manufacture of orthoformic acid alkylesters, Method of separating ethylene glycol and 1,2-butanediol, New environmentally-friendly process for synthetically separating lignocellulose from bagasse, Method for producing high-performance haydite from red mud, Method for separating lignin and cellulose from lignocellulose by using ionic liquid solvent, Method for preparing reducing sugar by catalyzing hydrocellulose, Preparation of cellulose and lignin by high boiling alcohol solvent, Biological asphalt and its preparation method, Carbon-based solid acid catalyst synthesized by one-step hydrothermal carbonization process, Combined process for preparing poly methoxy-dimethyl ether, Process for separating and recovering butyl acetate and butyl alcohol in wastewater by using azeotropic rectification, Separating and upgrading method of bio-oil by column chromatography, Method for preparing material rich in cellulose in degradable ionic liquid solvent, Method for recycling dichloromethane in acesulfame potassium synthesis process, Preparation technology of ethylene glycol terephthalate and preparation method of polyester, Enzymolysis xylogen or its derivative modified pnenolic aldehyde foam material and preparation method thereof, Method of extracting lignins different in molecular weight from bamboo pulping black liquor, Preparation method of hyperbranched polyester-polyvinyl alcohol pervaporation membrane, Method and equipment for recycling dimethylacetamide from waste pharmaceutical liquor and thermal coupling method, Solvent for separating biomass, and application thereof in selective separation of biomass, Composite solid base CaO-Al2O3 and method for preparing biodiesel oil by catalysis of waste vegetable oil with the same, Method for crystallization refinement of fluorine, Method with heat integration function for separating ethylene glycol from 1,2-butylene glycol, A kind of method of refining for bio oil multi-stage separation, Entry into force of request for substantive examination, Transfer of patent application or patent right or utility model.


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