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2-phenylpropionic acid one-pot synthesis method

A technology for phenylpropionic acid and phenylacetonitrile, which is applied in the field of one-pot synthesis of 2-phenylpropionic acid, can solve the problems of high cost, excessive solid waste, troublesome operation, etc., achieve good environmental protection and solve the effect of many operation steps

Inactive Publication Date: 2019-03-19
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The current production process of 2-phenylpropionic acid has the disadvantages of many solid wastes, long reaction steps, troublesome operation and high cost

Method used

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  • 2-phenylpropionic acid one-pot synthesis method

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Experimental program
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Effect test

Embodiment 1

[0041] Embodiment 1, a kind of method for synthesizing 2-phenylpropionic acid by one-pot method, carries out following steps successively:

[0042] Step 1), methylation reaction:

[0043] Add 58.5g (0.5mol) of phenylacetonitrile and 31.3g (0.58mol) of sodium methoxide into the reaction flask, and add 100ml of 30wt% sodium hydroxide aqueous solution into the tail gas absorption flask. The reaction was heated up to 180°C (i.e., the temperature of the control reaction flask was 180°C), and 90g (1mol) dimethyl carbonate was slowly added dropwise in the reaction flask (the addition time was 2h), and immediately the liquid evaporated and the gas (CO 2 ) is produced, and the distillate (mainly composed of dimethyl carbonate and methanol) is collected in the collection bottle, and the gas (CO 2 ) into the tail gas absorption bottle through the collecting bottle and be absorbed by the sodium hydroxide solution.

[0044] After the dimethyl carbonate has been added dropwise, take out t...

Embodiment 2～9

[0048] Change the mol ratio of phenylacetonitrile, sodium methylate, dimethyl carbonate in step 1) in embodiment 1, conditions such as reaction temperature, reaction time, all the other operations are identical to example 1, obtain embodiment 2~9, the result is as shown in table 1 .

[0049] Table 1

[0050]

[0051]

Embodiment 10～12

[0053] Change the sodium alkoxide of step 1) in the embodiment 1, the molar weight is constant; All the other are equal to embodiment 1, obtain embodiment 10~12; Results are shown in table 2.

[0054] Table 2

[0055] Example

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Abstract

The invention discloses a 2-phenylpropionic acid one-pot synthesis method. The 2-phenylpropionic acid one-pot synthesis method includes devices of a reaction flask, a collecting flask and a tail gas absorbing flask which are sequentially connected and comprises the following steps of 1) performing methylation reaction, specifically adding benzyl cyanide and sodium alkoxide into the reaction flask,filling carbon dioxide absorbent into the tail gas absorbing flask, controlling the temperature of the reaction flask to be 140-200 DEG C, slowly and dropwise adding dimethyl carbonate into the reaction flask, collecting vaporized gas-liquid mixtures from the reaction flask into the collecting flask, wherein gas in the gas-liquid mixtures is exhaust into the tail gas absorbing flask after passingthrough the collecting flask, after dropwise adding the dimethyl carbonate is completed, extracting the vaporized solution inside the collecting flask, distilling the vaporized solution to remove methyl alcohol, and then dropwise the distilled solution into the reaction flask to repeat the operations above; 2) filling water into the reaction flask for hydrolysis to obtain 2-phenylpropionic acid.The 2-phenylpropionic acid one-pot synthesis method has the advantages of being proper in reaction conditions and low in content of three wastes and production cost.

Description

technical field [0001] The invention relates to a method for synthesizing 2-phenylpropionic acid in one pot. Background technique [0002] 2-phenylpropionic acid, whose structural formula is shown in Formula 1, is widely used in the synthesis of medicines, spices and pesticides. [0003] [0004] At present, the industrial production of 2-phenylpropionic acid is mainly produced through methylation and hydrolysis of phenylacetonitrile. [0005] Document (Synthesis, 2018,50 (15): 2878-2886.) with phenylacetonitrile as raw material, methyl iodide as a methylation reagent, synthesized 2-phenylpropionitrile under the catalysis of lithium diisopropylamide, and then Hydrolysis under aqueous sodium hydroxide solution, and then acidification to obtain the product 2-phenylpropionic acid, the yield is 90%. This process uses the highly toxic methylation reagent methyl iodide, and produces solid waste of halogen salts. [0006] The literature (Chinese Journal of Pharmaceutical Indus...

Claims

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Application Information

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IPC IPC(8): C07C51/02C07C57/30
CPCC07C51/02C07C51/08C07C253/30C07C255/33C07C57/30
Inventor 陈新志张哲明阮诗想钱超
Owner ZHEJIANG UNIV
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