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.
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.
