Continuous flow synthesizing method and system for 4-chloro-3-oxo-ethyl butyrate without solvent

A solvent-free ethyl butyrate technology, applied in the field of solvent-free 4-chloro-3-oxo-butyric acid ethyl ester continuous flow synthesis, can solve the problems of non-environmental protection, cumbersome operation, and low product yield, and achieve Save production cost, increase yield and product content, and make the process green and environmentally friendly

Inactive Publication Date: 2018-04-17
NANTONG ACETIC ACID CHEM +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] In order to solve the above problems, the present invention provides a solvent-free 4-chloro-3-oxo-butyric acid ethyl ester continuous flow synthesis process, which has characteristics such as solvent-free and continuous synthesis, and its purpose is to solve the current The process of producing 4-chloro-3-oxo-butyric acid ethyl ester is not environmentally friendly, the product yield is low, the quality is poor, and the operation is cumbersome, etc.

Method used

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  • Continuous flow synthesizing method and system for 4-chloro-3-oxo-ethyl butyrate without solvent
  • Continuous flow synthesizing method and system for 4-chloro-3-oxo-ethyl butyrate without solvent
  • Continuous flow synthesizing method and system for 4-chloro-3-oxo-ethyl butyrate without solvent

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Embodiment 1

[0040]The invention provides a solvent-free 4-chloro-3-oxo-butyric acid ethyl ester continuous flow synthesis system, the solvent-free 4-chloro-3-oxo-butyric acid ethyl ester continuous flow synthesis method is applied to the system, the solvent-free 4-chloro-3-oxo-butyric acid ethyl ester continuous flow synthesis system includes a chlorine gas cylinder 1, the bottom of the chlorine gas cylinder 1 is connected to the top of the pressurized tank 5 through a pipeline, and the booster The upper end of pressure tank 5 is also connected with nitrogen cylinder 2, and the top of described booster tank 5 is connected with chlorination reaction module 8 through metering pump 7, and described chlorination reaction module 8 is also connected with diketene storage tank 9, and chlorination reaction The outlet of module 8 is connected with esterification reaction module 13, and described esterification reaction module 13 is also connected with ethanol storage tank 11 through metering pump 1...

Embodiment 2

[0046] Embodiment 2: a kind of solvent-free 4-chloro-3-oxo-butyric acid ethyl ester continuous flow synthetic method:

[0047] 1. describe with embodiment 1;

[0048] ②Open the pipeline shut-off valve 6, and the liquid chlorine and diketene 9 respectively pass through the metering pumps 7 and 10 and enter the reaction module 8 for chlorination reaction. The temperature of the chlorination reaction is -5°C, and the reaction time is 20s. The reaction molar ratio is 1.05:1;

[0049] ③After the chlorination reaction is finished, the ethanol in the ethanol storage tank 11 enters the reaction module 13 together with the chlorination solution through the metering pump 12, the temperature of the esterification reaction is 5°C, the reaction time is 15s, and the reaction molar ratio of ethanol to diketene is 1.02:1;

[0050] ④The crude product enters the gas-liquid separation buffer tank 15 after the pressure is relieved through the pressure gauge back pressure valve 14, and the tail ...

Embodiment 3

[0052] Embodiment 3: a kind of solvent-free 4-chloro-3-oxo-butyric acid ethyl ester continuous flow synthetic method:

[0053] 1. describe with embodiment 1;

[0054] ②Open the pipeline shut-off valve 6, liquid chlorine and diketene 9 respectively pass through the metering pumps 7 and 10 and enter the reaction module 8 at the same time for chlorination reaction. The temperature of the chlorination reaction is 15°C and the reaction time is 40s. The molar ratio is 1.1:1;

[0055] ③After the chlorination reaction is finished, the ethanol in the ethanol storage tank 11 enters the reaction module 13 together with the chlorination solution through the metering pump 12, the temperature of the esterification reaction is 25°C, the reaction time is 30s, and the reaction molar ratio of ethanol to diketene is 1.1:1;

[0056] ④The crude product enters the gas-liquid separation buffer tank 15 after the pressure is relieved through the pressure gauge back pressure valve 14, and the tail ga...

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Abstract

The invention belongs to the field of chemical engineering, and particularly relates to a continuous flow synthesizing method and a system for 4-chloro-3-oxo-ethyl butyrate without solvent. The methodcomprises the following steps of in the reaction process, firstly, performing chlorination reaction on diketene and liquid chloride through a micro-channel reactor module 8, and then performing esterification reaction on the chlorinating liquid and ethyl alcohol through a reaction module 13, so as to obtain a crude product of the 4-chloro-3-oxo-ethyl butyrate; performing pressure-relief rectification on the crude product, so as to obtain a finished product of the 4-chloro-3-oxo-ethyl butyrate. The method can solve the problem that because the micro-channel reactor has certain drag, the liquidchloride cannot be fed by a conventional feeding device; in the micro-channel reactor, the mixing effect of gas and liquid reaction is poorer than the mixing effect of liquid and liquid reaction, themetering accuracy of gas is poor, the amount of reaction byproducts is increased, the yield rate is reduced, and the like.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a solvent-free 4-chloro-3-oxo-butyric acid ethyl ester continuous flow synthesis method and system. Background technique [0002] 4-Chloro-3-oxo-butyric acid ethyl ester is a colorless light yellow liquid, molecular weight: 164.59, melting point: -8℃, boiling point: 115℃14mmHg, density: 1.218, flash point: 96℃, water solubility: 47.5g / L (20°C). 4-Chloro-3-oxo-butyric acid ethyl ester is a good intermediate for pharmaceutical synthesis, mainly used to produce oxiracetam, oxiracetam belongs to the drug for the treatment of cerebrovascular diseases, it is the fourth generation benefit Smart drugs, derivatives of pyrrolidones, the trade names are Jianlangxing, Ou Laining, neuromet and neupan, etc. Oxiracetam is a new type of central nervous system drug, which can promote the functional recovery of nerve cells and improve brain metabolism. It has multiple functions, has...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/58C07C59/21C07C67/14C07C67/54C07C69/72B01J19/00
CPCB01J19/0093C07C51/58C07C67/14C07C67/54C07C59/21C07C69/72
Inventor 庆九俞新南薛金全朱小刚刘芳卢乐朱爱华
Owner NANTONG ACETIC ACID CHEM
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