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A kind of method for continuously preparing cyclopropylamine

A technology for cyclopropylamine and cyclopropylformamide, which is applied in the field of continuous preparation of cyclopropylamine, can solve the problems of difficult effective control of the reaction process, slow reaction rate, high equipment requirements, etc., and achieve high product yield, short reaction cycle, and low equipment investment Effect

Active Publication Date: 2020-10-16
深圳智微通科技有限公司
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  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

This kind of process has greater requirements on the distillation capacity of the rectification tower, and two rectification towers are required to cooperate to achieve a satisfactory separation effect, and there will be obvious back-mixing in the rectification tower, and the reaction process is difficult. Effective control
Although the above process makes the cyclopropanamide Hoffman rearrangement process continuous, there are still low-temperature reaction stages with slow reaction rate and long reaction time, relatively high equipment requirements, and no real enhancement of the reaction process.

Method used

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  • A kind of method for continuously preparing cyclopropylamine

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Comparison scheme
Effect test

Embodiment 1

[0029] as per figure 1 Shown process continuously prepares cyclopropylamine:

[0030] (1) Preparation of solution A: Add 75g of water to 22g of cyclopropanamide, and dissolve it in a water bath at 40°C under temperature control and stirring, then dilute to 100mL with water to prepare a solution with a density of cyclopropanamide solution close to 1 A;

[0031] (2) Prepare solution B: under temperature control and stirring in a water bath at 10-20°C, slowly add 23.5g of sodium hydroxide solid to 186g of sodium hypochlorite solution with an available chlorine content of 10.1%, add a small amount of water, dissolve it, and then add water Dilute to 160mL, prepare solution B;

[0032] (3) The solution A obtained in step (1) and the solution B obtained in step (2) are continuously passed into the micro-reaction equipment at a flow rate of 5mL / min and 8mL / min respectively, and the micro-reaction equipment mainly consists of a 40°C micro-sieve reactor and Composed of 90°C temperatu...

Embodiment 2

[0035] as per figure 1 Shown process continuously prepares cyclopropylamine:

[0036] (1) Preparation of solution A: add 70 g of water to 25 g of cyclopropanamide, dissolve in a water bath at 40°C with temperature control and stirring, and then dilute to 100 mL with water to prepare solution A;

[0037] (2) Prepare solution B: under temperature control and stirring in a water bath at 10-20°C, slowly add 25.9g of sodium hydroxide solid to 175g of sodium hypochlorite solution with an available chlorine content of 12.5%, and add a small amount of water to dissolve it, then water Dilute the volume to 200mL, and prepare solution B;

[0038] (3) The solution A obtained in step (1) and the solution B obtained in step (2) are continuously passed into the micro-reaction equipment at a flow rate of 5mL / min and 10mL / min respectively, and the micro-reaction equipment mainly consists of a 40°C membrane dispersion microreactor and Composed of 80°C temperature-controlled coils; the two sol...

Embodiment 3

[0041] as per figure 1 Shown process continuously prepares cyclopropylamine:

[0042] (1) Preparation of solution A: add 68 g of water to 30 g of cyclopropanamide, dissolve in a water bath at 50°C under temperature control and stirring, and then dilute to 100 mL with water to prepare solution A;

[0043] (2) Prepare solution B: under temperature control and stirring in a water bath at 20-30°C, slowly add 36.7g of sodium hydroxide solid to 216g of sodium hypochlorite solution with an available chlorine content of 12.5%, and add a small amount of water to dissolve it, and then add water Dilute to 250mL, prepare solution B;

[0044] (3) The solution A obtained in step (1) and the solution B obtained in step (2) are continuously passed into the micro-reaction equipment at a flow rate of 5mL / min and 12.5mL / min respectively, and the micro-reaction equipment is mainly composed of a 60°C membrane dispersion microreactor and 70°C temperature control coil; the two solutions are quickl...

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Abstract

The invention discloses a method for continuous preparation of cyclopropylamine and belongs to the technical field of chemical production. Specifically, the method comprises the following steps: (1) dissolving cyclopropyl carboxamide in water to prepare a solution A; (2) mixing sodium hypochlorite, sodium hydroxide and water to prepare a solution B; (3) continuously introducing the solution A andthe solution B into a micromixer and mixing to obtain a reaction liquid C, and letting the reaction liquid C enter a tubular reactor and reacting; (4) rectifying the material obtained in the Step (3)to obtain cyclopropylamine. Only through one-step high temperature reaction, the cyclopropylamine can be separated by a rectification device, and yield of cyclopropylamine reaches 94% and above. The method is efficient and economic and helps solve problems of existing technologies, such as cumbersome process, low production efficiency and unstable products, etc.

Description

technical field [0001] The invention belongs to the technical field of chemical production, in particular to a method for continuously preparing cyclopropylamine. Background technique [0002] Cyprofloxacin is an essential intermediate for the production of fluoroquinolone antibacterial drugs such as ciprofloxacin and gatifloxacin, and it can also be used in the synthesis of plant protection agents and feed additives. The application of cyclopropylamine is very extensive. With the development and application of downstream products, it has a very large market prospect in the field of medicine and organic synthesis. [0003] The Hofmann rearrangement reaction is the final reaction step in the process of synthesizing cyclopropylamine. Although many improved conditions such as lead tetraacetate, N-bromosuccinimide, and hypervalent iodine reagents have been developed for the Hoffman rearrangement reaction, sodium hydroxide is still mainly used in industry due to economic factors...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/62C07C209/58C07C211/35
Inventor 徐建鸿黄晋培耿宇昊
Owner 深圳智微通科技有限公司