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Preparation method of 2-chloroacetoacetic acid ethyl ester

A technology of ethyl chloroacetoacetate and ethyl acetoacetate, which is applied in the field of preparation of pharmaceutical intermediates, can solve problems such as large amount of waste water, low yield of ethyl 2-chloroacetoacetate, and inability to treat waste COD acid, and achieve The effect of high yield

Inactive Publication Date: 2015-03-25
SHANDONG HUIHAI PHARMA & CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The technical problem to be solved by this invention is to provide a kind of preparation method of ethyl 2-chloroacetoacetate, more exactly a kind of green economic synthesis and separation of ethyl 2-chloroacetoacetate and by-product hydrogen chloride and sulfur dioxide The method overcomes the problems such as the low yield of ethyl 2-chloroacetoacetate, the large amount of waste water, and the inability to handle high COD waste acid in the prior art

Method used

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  • Preparation method of 2-chloroacetoacetic acid ethyl ester
  • Preparation method of 2-chloroacetoacetic acid ethyl ester

Examples

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Embodiment 1

[0024] Add 130kg of ethyl acetoacetate to the reaction kettle, add 135kg of sulfuryl chloride (1.03 times) dropwise within 2 hours at room temperature, keep the temperature in the chlorination kettle at 80-100°C during the dropping process, and keep the vacuum at -0.3-0.35MPa , the hydrogen chloride and sulfur dioxide gases generated in the reaction are introduced into the oxidation deacidification tower by vacuum, and the oxidation deacidification tower is turned on to spray, the oxidation temperature is controlled at 55-65°C, the pressure is -0.02--0.05MPa, and 400kg (3.1 times, 20 %) sulfur dioxide generated by the oxidation of hydrogen peroxide. After the sulfuryl chloride was added dropwise, the chlorination kettle was kept at 80-100°C for 2 hours. After the heat preservation was completed, 360kg (10.1%) of hydrochloric acid and 140kg (69.8%) of sulfuric acid were distilled at 100-110°C. After the crude product was rectified, 153.8 kg of ethyl 2-chloroacetoacetate was obt...

Embodiment 2

[0026] Add 130kg of ethyl acetoacetate to the reaction kettle, add 149kg of sulfuryl chloride (1.15 times) dropwise within 2 hours at room temperature, keep the temperature in the chlorination kettle at 80-100°C during the dropping process, and keep the vacuum at -0.3-0.5MPa , the hydrogen chloride and sulfur dioxide gases generated in the reaction are introduced into the oxidation deacidification tower by vacuum, and the oxidation deacidification tower is turned on to spray, the oxidation temperature is controlled at 45-60°C, the pressure is -0.02--0.05MPa, and 300kg (2.3 times, 20 %) sulfur dioxide generated by the oxidation of hydrogen peroxide. After the sulfuryl chloride was added dropwise, the chlorination kettle was kept at 80-100°C for 1 hour. After the heat preservation was completed, 240kg (15.2%) of hydrochloric acid and 158kg (62%) of sulfuric acid were distilled at 100-110°C. After the crude product was rectified, 153kg of ethyl 2-chloroacetoacetate was obtained, ...

Embodiment 3

[0028] Add 130kg of ethyl acetoacetate to the reaction kettle, add 140kg (1.07 times) of sulfuryl chloride dropwise within 2 hours at room temperature, keep the temperature in the chlorination kettle at 80-100°C during the dropping process, and keep the vacuum at -0.4-0.5MPa , the hydrogen chloride and sulfur dioxide gases generated in the reaction are introduced into the oxidation deacidification tower by vacuum, and the oxidation deacidification tower is turned on to spray, the oxidation temperature is controlled at 65-75 °C, the pressure is -0.02--0.05MPa, and 65kg (0.5 times, 20 %) sulfur dioxide generated by the oxidation of hydrogen peroxide. After the sulfuryl chloride was added dropwise, the chlorination kettle was kept at 80-100°C for 2 hours. After the heat preservation was completed, 180kg (20.3%) of hydrochloric acid and 116kg (84.5%) of sulfuric acid were distilled at 100-110°C. After the crude product was rectified, 155.1 kg of ethyl 2-chloroacetoacetate was obta...

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Abstract

The invention discloses a preparation method of 2-chloroacetoacetic acid ethyl ester. The preparation method comprises the following step: with acetoacetic acid ethyl ester as a starting raw material, performing separation on sulfur dioxide and hydrogen chloride by virtue of four steps namely chlorination, a step of producing dilute sulfuric acid by oxidizing sulfur dioxide by virtue of oxidative deacidification, hydrochloric acid distillation and rectification to obtain 2-chloroacetoacetic acid ethyl ester. Compared with the prior art, the preparation method disclosed by the invention has the advantages that 1, complete separation between hydrogen chloride and sulfur dioxide can be achieved by virtue of an oxidative deacidification technology; 2, high-quality sulfuric acid and hydrochloric acid can be produced as byproducts, and certain economic benefits can be generated; and 3, a process for removing sulfur dioxide and hydrogen chloride by virtue of water washing in a conventional 2-chloroacetoacetic acid ethyl ester synthesis process can be replaced, and energy conservation and environmental protection can be achieved.

Description

technical field [0001] The invention relates to a preparation method of a pharmaceutical intermediate, in particular to a preparation method of ethyl 2-chloroacetoacetate. Background technique [0002] Ethyl 2-chloroacetoacetate is a colorless to light yellow transparent liquid, which is mainly used in the field of medicine, especially the key intermediate for the synthesis of cefodizime, and has broad market prospects. [0003] After finding relevant information and comparative analysis, there are mainly two processing routes for synthesizing ethyl 2-chloroacetoacetate both at home and abroad at present, as follows: [0004] 1. Chlorine gas method: Chlorination is carried out with chlorine gas as the chlorination agent. Because the chlorine gas molecules are too active, the 2-position and 4-position of ethyl acetoacetate can be chlorinated, and the conversion rate is equal, so the obtained It is a mixture of ethyl 2-chloroacetoacetate and ethyl 4-chloroacetoacetate, and th...

Claims

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Application Information

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IPC IPC(8): C07C69/72C07C67/32
CPCC07C67/307C01B7/0706C01B17/775C07C69/716
Inventor 牟应科郑庚修张世凤张忠政姜福元王乐强于西波
Owner SHANDONG HUIHAI PHARMA & CHEM
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