Trimethyl orthoacetate synthesis
- Product Name:Trimethyl orthoacetate
- CAS Number:1445-45-0
- Molecular formula:C5H12O3
- Molecular Weight:120.15
Trimethyl orthoacetate is an intermediate for the production of medicines and pesticides, as well as the main raw material for the production of food additives, coatings, paints, etc. The preparation method is as follows: anhydrous acetonitrile, methanol and carbon tetrachloride are introduced into the metered dry HCl gas at -10°C. Then, the reaction was stirred at 0-5° C. for 12 h to obtain a reaction mixture of crude imino ether hydrochloride, which was then purified with 28% sodium methoxide methanol solution to obtain trimethyl orthoacetate with a yield of 90%.
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Yield:1445-45-0 95.16%
Reaction Conditions:
Stage #1:methanol;acetonitrile with hydrogenchloride;cetyltrimethylammonium chloride in hexane at -10; for 6 h;Large scale;
Stage #2:methanol; pH=5-6 at 40; for 4 h;Large scale;Reagent/catalyst;Temperature;
Steps:
1 Example 1
1) With a stirrer,Temperature probe of 1.5m high 1000L enamel reactor,The reactor was charged with 82 kg of acetonitrile,Anhydrous methanol 67.2kg and 300kg n-hexane, the reaction solution was cooled to -10 ° C,While stirring, 0.085 kg of a water-absorbing surfactant cetyltrimethylammonium chloride was added,85 kg of dry hydrogen chloride gas was slowly introduced,And then fully agitated reaction completed 6 hours into salt,To give alkyliminoacetate hydrochloride. 2) In step 1)The resulting alkyliminoacetate hydrochloride salt was charged with 160 kg of anhydrous methanol,And the PH value of the reaction liquid is regulated to 5.5 to 6.0.The reaction mixture was stirred at 40 ° C for 4 hours to complete the alcoholysis.Cooling filtration desalination,The filtrate was distilled to obtain trimethyl orthoacetate 233kg, content 98.02%, yield 95.16%.
References:
Jiangsu Yangnong Chemical Co., Ltd.;Jiangsu Youshi Chemical Co., Ltd;Wang, Dongchao;Yang, Fan;Kong, Yong;Jie, Chunman;Guo, Yubo CN105384614, 2016, A Location in patent:Paragraph 0024; 0025; 0026; 0045; 0046
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