Continuous flow synthesizing method and system for methyl 4-chloroacetoacetate without solvent

A technology of methyl acetate and chloroacetyl, which is applied to the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of acyl halides. It can solve the problems of cumbersome operations, poor quality, and low product yields, and achieve high yield and product content. Improve, save production cost, and process green environmental protection effect

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

[0008] In order to solve the above problems, the invention provides a solvent-free 4-chloroacetoacetate continuous flow synthesis method and system, which has characteristics such as solvent-free and continuous synthesis, and its purpose is to solve the problem of the current production of 4-chloroacetoacetate methyl ester The process 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 methyl 4-chloroacetoacetate without solvent
  • Continuous flow synthesizing method and system for methyl 4-chloroacetoacetate without solvent
  • Continuous flow synthesizing method and system for methyl 4-chloroacetoacetate without solvent

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Embodiment 1

[0042] Embodiment 1: a kind of solvent-free 4-chloroacetoacetate methyl ester continuous flow synthetic method:

[0043] ① Open the valve of the inverted chlorine cylinder 1, and open the pipeline shut-off valve 3 to release the liquid chlorine and introduce it into the liquid chlorine pressurized tank 5. After the liquid level reaches 2 / 3, close the valve of the chlorine cylinder 1 and the shut-off valve 3, and open Nitrogen cylinder 2 valve and pipeline shut-off valve 4 pressurize the pressurized tank;

[0044] ② Open 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 for chlorination reaction, the temperature of the chlorination reaction is -25°C, the reaction time is 5s, the liquid chlorine and diketene The reaction molar ratio is 1:1;

[0045] ③After the chlorination reaction, the methanol in the methanol storage tank 11 enters the reaction module 13 together with the chlorin...

Embodiment 2

[0048] Embodiment 2: a kind of solvent-free 4-chloroacetoacetate methyl ester continuous flow synthesis method:

[0049] 1. describe with embodiment 1;

[0050] 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;

[0051] ③ After the chlorination reaction is finished, the methanol in the methanol 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 methanol to diketene is 1.03:1;

[0052] 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...

Embodiment 3

[0054] Embodiment 3: a kind of solvent-free 4-chloroacetoacetate methyl ester continuous flow synthesis method:

[0055] 1. describe with embodiment 1;

[0056] 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 for chlorination reaction, the temperature of the chlorination reaction is 15°C, and the reaction time is 35s. The molar ratio is 1.1:1;

[0057] ③After the chlorination reaction is finished, the methanol in the methanol 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 28°C, the reaction time is 30s, and the reaction molar ratio of methanol to diketene is 1.15:1;

[0058] 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 gas enters the absor...

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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 methyl 4-chloroacetoacetate without solvent. The method comprises 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 methyl alcohol through a reaction module 13, so as to obtain a crude product of the methyl 4-chloroacetoacetate; performing pressure-relief rectification on the crude product, so as to obtain a finished product of the methyl 4-chloroacetoacetate. The method can solve the problem that because the micro-channel reactor has certain drag, the liquid chloride 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, the metering 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 continuous flow synthesis method and system of methyl 4-chloroacetoacetate. Background technique [0002] Methyl 4-chloroacetoacetate is a colorless light yellow liquid, molecular weight: 150.56, melting point: 14-16°C, boiling point: 212°C, density: 1.287, flash point: 107°C, water solubility: 71g / L (20°C ). Methyl 4-chloroacetoacetate is a good pharmaceutical synthesis intermediate, mainly used to produce oxiracetam, oxiracetam belongs to the drug for the treatment of cerebrovascular diseases, is the fourth generation of nootropic drugs, pyrrolidones Derivatives, 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 significant curative effect on treating amn...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/58C07C59/21C07C67/14C07C67/54C07C69/72B01J19/00B01J4/00
CPCB01J4/001B01J19/0093B01J2219/00867B01J2219/00891C07C51/58C07C67/14C07C67/54C07C59/21C07C69/72
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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