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A kind of method of synthetic cyanoacetate

A technology of cyanoacetate and cyanoacetic acid is applied in the field of catalyzing the esterification of cyanoacetic acid and alcohol, and can solve problems such as reports on general methods for cyanoacetate compounds, and achieve low energy loss, short reaction time, The effect of simple reaction operation and process

Inactive Publication Date: 2015-09-16
浙江久而久化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

People such as Qiu Tao disclose a kind of hydrotalcite or hydrotalcite-like as catalyst, catalyze methyl cyanoacetate and ethanol to carry out the process method (publication number CN 101245034A) of esterification exchange method to synthesize ethyl cyanoacetate, the people such as Douglas J.Raber reported that cyanoacetic acid and alkylating reagent [Et 3 O] + BF 4 3+ The method (Journal of Organic Chemistry, 44 (7), 1149-54; 1979) of reaction synthesis ethyl cyanoacetate, has not yet seen the report of the general method for preparing a series of cyanoacetate compounds about new type, environmental protection, green

Method used

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  • A kind of method of synthetic cyanoacetate
  • A kind of method of synthetic cyanoacetate
  • A kind of method of synthetic cyanoacetate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 3.02g (10mmol) ionic liquid [(CH 2 ) 3 SO 3 Hmin] HSO 4 Put 4.339g (50mmol) cyanoacetic acid and 1.6g (50mmol) methanol into a reaction flask, stir, heat, control the temperature at 60°C, and react for 4h. The lower esterification product, methyl cyanoacetate, was qualitatively and quantitatively analyzed by GC-MS to obtain a yield of 80.36%. The ionic liquid layer is reused after water extraction, washing, heating and dehydration under reduced pressure, and removal of organic matter.

Embodiment 2

[0026] 3.02g (10mmol) ionic liquid [(CH 2 ) 3 SO 3 Hmin] HSO 4 Put 4.339g (50mmol) cyanoacetic acid and 2.3g (50mmol) ethanol into a reaction flask, stir, heat, control the temperature at 80°C, react for 4h, let the reaction solution stand still, separate layers, and separate the upper layer through liquid separation for esterification The product, ethyl cyanoacetate, was qualitatively and quantitatively analyzed by GC-MS and the yield was 79.05%. The ionic liquid layer is reused after being extracted and washed with water, dehydrated under reduced pressure by heating, and removing organic matters.

Embodiment 3

[0028] 3.02g (10mmol) ionic liquid [(CH 2 ) 3 SO 3 Hmin] HSO 4 Put 4.339g (50mmol) cyanoacetic acid and 3g (50mmol) n-propanol into a reaction flask, stir, heat, control the temperature at 80°C, react for 4h, let the reaction solution stand still, separate layers, and separate the upper ester through liquid separation The product propyl cyanoacetate was qualitatively and quantitatively analyzed by GC-MS to obtain a yield of 81.32%. The ionic liquid layer is reused after being extracted and washed with water, dehydrated under reduced pressure by heating, and removing organic matters.

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Abstract

A method for synthesizing cyanoacetate. Cyanoacetic acid is catalyzed to react with alcohol in an esterification reaction to obtain cyanoacetate; the method is characterized in that ionic liquid is used as a reaction medium and a catalyst of the esterification reaction; the ionic liquid is selected from one of the following molecular structural formulae, such as imidazole ionic liquid in molecular structural formula I-1, pyrrolidone ionic liquid in molecular structural formula I-2, or pyridine sulfonic acid ionic liquid in molecular structural formula I-3; compared with a traditional concentrated sulfuric acid catalytic method, the method of the invention has the advantages of simple operation, easy product separation, capability of ionic liquid recycle, environment friendliness and the like, and has very good industrial application prospects; wherein, R1 is H or a sulfopropyl group; X is HSO4, or BF4.

Description

technical field [0001] The invention relates to a method for catalyzing the esterification reaction of cyanoacetic acid and alcohol in organic chemical reaction methods. Background technique [0002] Cyanoacetate compounds are important raw materials for organic synthesis and intermediates of pharmaceutical dyes, especially ethyl cyanoacetate, as an important chemical intermediate, is mainly used to synthesize instant adhesive 502 glue. It undergoes a condensation reaction with formaldehyde under the action of a basic catalyst, and obtains a-cyanoacrylate ethyl ester monomer through dehydration, drying, cracking and vacuum distillation. [0003] Existing methods for preparing cyanoacetates include sulfuric acid catalyzed method (Journal of Agricultural and Food Chemistry, 58 (5), 2730-2735; 2010), the method of organic solvent as water-carrying agent (Faming Zhuanli Shenqing, 101544669, 30 Sep 2009), and the method of adding a dehydrating agent (European Journal of Organic ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C255/19C07C253/30
Inventor 陈金才张婷婷梁洪泽余波姚江
Owner 浙江久而久化学有限公司