1445-45-0Relevant articles and documents
Process for producing high-quality trimethyl orthoacetate
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Paragraph 0014; 0015; 0016; 0017; 0018; 0019, (2018/04/21)
The invention discloses a process for producing high-quality trimethyl orthoacetate. The process comprises the steps of: in the presence of a pseudocumene solvent, performing a salt-forming reaction on acetonitrile, methanol and hydrogen chloride to prepare ethylenediamine methyl ether hydrochloride, then putting the obtained ethylenediamine methyl ether hydrochloride in a methanol solution, adding an ammonium methanol solution dropwise so as to adjust the pH value, performing an alcoholysis reaction to obtain a crude product of trimethyl orthoacetate, performing filtration so as to remove solid ammonium chloride for recycling, performing adsorption on the obtained filtrate by using strongly alkaline macroporous ion exchange resin so as to remove chloride ions, and finally performing continuous rectification to obtain the trimethyl orthoacetate product which has a content of more than 99.5% and a yield of more than 85%. The process is simple, the product is stable and reliable, the adopted pseudocumene solvent has low toxicity and is safe to use.
Production process of high-quality trimethyl orthoacetate
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Paragraph 0016; 0017; 0019, (2017/08/29)
The invention discloses a production process of high-quality trimethyl orthoacetate. The production process comprises the following steps: performing salification reaction on acetonitrile, methanol and chlorine hydride in the presence of a solvent unsym-trimethyl benzene, so as to obtain ethyleneimine methyl ether hydrochloride; then adding the ethyleneimine methyl ether hydrochloride into a methanol solution; dropwise adding an aminomethanol solution to regulate a pH value, performing alcoholysis reaction to obtain a trimethyl orthoacetate crude product; filtering out solid ammonium chloride, and recycling the solid ammonium chloride; adsorbing filtrate by use of strong-basicity macroporous ion-exchange resin so as to remove chloridion; and finally performing continuous rectification, thereby obtaining a trimethyl orthoacetate product with content greater than 999.5% and yield greater than 85%. The production process is simple in process, the product is stable and reliable, and the used unsym-trimethyl benzene solvent is low in toxicity and safe to use.
A hydrogen chloride producing toluene diisocyanate methyl-acetate production method
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Paragraph 0047-0060, (2017/02/24)
The invention discloses a method for producing trimethyl orthoacetate by utilizing hydrogen chloride (HCl) generated during production of toluene diisocynate (TDI). The method comprises the following steps: carrying out pressure boosting on a dried normal-pressure and low-temperature HCl waste gas taken as a byproduct during production of TDI and then feeding methyl alcohol into HCl so as to prepare an alcohol acid; carrying out a salt forming reaction on the alcohol acid and acetonitrile in an inert solvent so as to prepare an ethyleneimine methyl ether hydrochloride; feeding methyl alcohol twice, carrying out an alcoholysis reaction and distilling so as to prepare trimethyl orthoacetate. According to the method, dried normal-pressure and low-temperature HCl generated during the production of TDI is taken a raw material, namely, the recycling of a waste material is realized, so that the cost is lowered; the safety and the environmental friendliness are realized. The alcohol acid is prepared, so that the problems that the metering of HCl is inaccurate and the temperature is difficult to control because a large quantity of heat is released during the salt forming reaction are solved; the solvent with a high boiling point is used, so that the safe and environment-friendly problem that the solvent with a low boiling point is toxic and flammable is solved; the continuous rectification is carried out, so that the problem of long production cycle is solved. The yield of prepared trimethyl orthoacetate can reach 76% to 80%.
Trimethyl orthoacetate synthesis method
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Paragraph 0024; 0025; 0026; 0045; 0046, (2016/10/20)
The present invention provides a trimethyl orthoacetate synthesis method, wherein acetonitrile and methanol are adopted as starting raw materials. The method comprises: 1) when acetonitrile, methanol and a non-polar solvent are subjected to mixing cooling in a reaction kettle to achieve a temperature of -20 to -5 DEG C, adding a small amount of a Gemini surfactant to the system, then introducing dried hydrogen chloride gas to make a molar ratio of acetonitrile to methanol to hydrogen chloride to the surfactant be 1:1-2:1.05-1.5:0.001-0.005 and make a mass ratio of acetonitrile to the non-polar solvent be 1:2-5, and carrying out a complete stirring reaction after introducing the hydrogen chloride gas so as to generate an ethylenediamine methyl ether hydrochloride; and 2) adding methanol having the amount 2-4 times the molar amount of the starting acetonitrile is added to the ethylenediamine methyl ether hydrochloride generated in the step 1), adjusting the pH value of the reaction system to 5-6.5, carrying out an alcoholysis reaction at a temperature of 25-40 DEG C, filtering the alcoholysis product, and refining to obtain the trimethyl orthoacetate. With the method of the present invention, the water content of the original ester synthesis system can be completely reduced so as to significantly improve the trimethyl orthoacetate yield.
Orthoester exchange: A tripodal tool for dynamic covalent and systems chemistry
Brachvogel, Ren-Chris,Von Delius, Max
, p. 1399 - 1403 (2015/02/05)
Reversible covalent reactions have become an important tool in supramolecular chemistry and materials science. Here we introduce the acid-catalyzed exchange of O,O,O-orthoesters to the toolbox of dynamic covalent chemistry. We demonstrate that orthoesters readily exchange with a wide range of alcohols under mild conditions and we disclose the first report of an orthoester metathesis reaction. We also show that dynamic orthoester systems give rise to pronounced metal template effects, which can best be understood by agonistic relationships in a three-dimensional network analysis. Due to the tripodal architecture of orthoesters, the exchange process described herein could find unique applications in dynamic polymers, porous materials and host-guest architectures.
Divergent Diels-Alder methodology from methyl coumalate toward functionalized aromatics
Lee, Jennifer J.,Kraus, George A.
supporting information, p. 2366 - 2368 (2013/06/26)
An inverse electron-demand Diels-Alder reaction between methyl coumalate and electron-rich dienophiles produces substituted benzoates. A high-yielding, single-pot procedure transforms readily accessible vinyl ether, ketal, or orthoester dienophiles into functionalized aromatic systems in a versatile route.
METHOD FOR PRODUCING IMIDE ETHER COMPOUND
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Page/Page column 21-22; 24; 3/4, (2008/06/13)
A method for producing an imide ether compound in high yield is provided. The method is characterized in that a nitrile compound, an alcohol and a hydrogen halide are continuously introduced into a flow reaction apparatus comprising a mixing vessel and a flow reactor, to react them with one another. Since the reaction proceeds with 1 : 1 by the use of a flow reactor, an improved selectivity is achieved and the formation of a by-product is reduced, which results in the efficient production of an imide ether compound.
New phenylalanine derivatives
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, (2008/06/13)
Specified phenylalanine derivatives and analogues thereof have an antagonistic activity to α4 integrin. They are used as therapeutic agents for various diseases concerning α4 integrin.
Influence of Solvent and Counterion in the Reactions of Alkoxide Ions with the 2-Nitropropan-2-yl Radical
Russel, Glen A.,Baik, Woonphil
, p. 196 - 198 (2007/10/02)
Photostimulated free radical chain reactions between alkoxide ions derived from primary alcohols and XCMe2NO2 (X= Cl, Br, NO2, PhSO2, N3, or p-ClC6H4S) occur to produce Me2C(OR)2 by reaction involving the trapping of Me2C(NO2). by RO-, the decomposition of ROCMe2NO2.- to ROCMe2., and the oxidation of ROCMe2. to Me2C=OR+ by XCMe2NO2.