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Method for preparing ethyl propiolate by one-pot method

A technology of ethyl propiolate and diethyl carbonate, which is applied in the field of one-pot preparation of ethyl propiolate, can solve the problems of difficult industrial production, low product yield, complicated preparation process, etc., and achieves a simple and efficient preparation method. The post-treatment process is simple, and the effect of improving yield and purity

Pending Publication Date: 2021-12-28
杭州盛弗泰新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention aims to overcome the problems of complex preparation process, low product yield and difficulty in industrialized production in the method for preparing ethyl propiolate through the esterification reaction of propiolic acid and acetic acid in the prior art, and provides a one-pot method The method for preparing ethyl propiolate is to prepare ethyl propiolate through the reaction of sodium propiolate and diethyl carbonate, the preparation method is simple, the amount of waste water is less, the product with high yield and high purity can be obtained, and it is suitable for industrialization Production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A kind of one-pot method prepares the method for ethyl propiolate, comprises the steps:

[0029] (1) 112g (2mol) propynyl alcohol, 1.6g ferrous chloride catalyst and 100g water were added in the reactor, stirred and mixed to obtain the reaction solution, and the temperature in the reactor was maintained at 20°C;

[0030] (2) dripping 906g mass concentration of 30% hydrogen peroxide in the reaction solution with a dropping funnel, the time of dropping is 2h, and the pH value of the system is controlled between 4 to 5 with saturated sodium bicarbonate solution in the dropping process, and kept The temperature of the reaction kettle is at 20°C; after the dropwise addition, heat-preserve and stir at 20°C for 3 hours, then take a sample for testing, so that the reaction of propynyl alcohol is completed; then slowly raise the temperature to 60°C within 2 hours, and continue the heat-retaining reaction until the reaction solution is uniform Transparent;

[0031] (3) Add 5 g o...

Embodiment 2

[0034] A kind of one-pot method prepares the method for ethyl propiolate, comprises the steps:

[0035] (1) Add 112g (2mol) propynyl alcohol, 3g cuprous chloride catalyst and 100g water into the reactor, stir and mix to obtain the reaction solution, and keep the temperature in the reactor at 15°C;

[0036] (2) dripping 1020g mass concentration is 30% hydrogen peroxide in reaction solution with dropping funnel, time of dropping 1.5h, control system pH value between 4~5 with saturated sodium bicarbonate solution in the dropping process, and Keep the temperature of the reaction kettle at 15°C; after the dropwise addition, first heat and stir the reaction at 15°C for 3.5 hours, take a sample for detection, and make the reaction of propynyl alcohol complete; then slowly raise the temperature to 65°C within 2 hours, and continue the heat preservation reaction until the reaction liquid Uniform and transparent;

[0037] (3) Add 5.6g of HZSM-5 molecular sieve (Jiangsu Xianfeng Nano Ma...

Embodiment 3

[0040] A kind of one-pot method prepares the method for ethyl propiolate, comprises the steps:

[0041] (1) 112g (2mol) propynyl alcohol, 2g ferrous chloride catalyst and 100g water are added in the reactor, stirred and mixed to obtain the reaction solution, and the temperature in the reactor is maintained at 25°C;

[0042] (2) dropwise adding 800g of mass concentration in the reaction solution with a dropping funnel is 30% hydrogen peroxide and 2.5h for the time of dropping, and the pH value of the system is controlled between 4 to 5 with saturated sodium bicarbonate solution in the dropping process, And keep the temperature of the reaction kettle at 25°C; after the dropwise addition, first heat and stir the reaction at 25°C for 2.5 hours, take a sample for detection, and make the reaction of propynyl alcohol complete; then slowly raise the temperature to 70°C within 2 hours, and continue the heat preservation reaction until the reaction The liquid is uniform and transparent;...

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Abstract

The invention relates to the field of preparation of organic chemical industry raw materials, and discloses a method for preparing ethyl propiolate by a one-pot method. The methodcomprises the following steps: (1) adding sodium bicarbonate and a catalyst into water, and mixing to obtain a reaction solution; (2) dropwise adding hydrogen peroxide and propargyl alcohol into the reaction solution for reaction; (3) adding a molecular sieve into the reacted solution, and then dropwise adding diethyl carbonate for reaction; and (4) after the reaction is finished, separating to obtain an organic phase, spin-drying the organic phase, and rectifying to obtain an ethyl propiolate product. According to the invention, ethyl propiolate is prepared through a reaction of sodium propiolate and diethyl carbonate, the preparation method is simple, the amount of waste water is small, the high-yield and high-purity product can be obtained, and the method is suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of preparation of organic chemical raw materials, in particular to a method for preparing ethyl propiolate in one pot. Background technique [0002] Ethyl propiolate is an important organic chemical raw material and pharmaceutical intermediate. Ethyl propiolate is obtained by the esterification reaction of propiolic acid and ethanol under the effect of catalyst in the prior art, and there are following problems in the preparation process: 1, product separation difficulty, easily form azeotrope with alcohol or solvent, The yield is generally low, generally below 60%; 2, because the product is highly irritating, the operating environment for workers is poor, and the cost of raw materials is high, the post-treatment process is complicated, and there is no advantage in cost, so it is difficult to industrialize production. [0003] The Chinese patent literature with the notification number CN101318900B discloses...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/40C07C69/606
CPCC07C67/40C07C69/606Y02P20/584
Inventor 刘文龙
Owner 杭州盛弗泰新材料科技有限公司
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