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Synthesis method of N-methyl isopropylamine

A technology of methyl isopropylamine and a synthesis method, which is applied in the field of preparation of N-methyl isopropylamine, can solve the problems of serious equipment corrosion, poor product selectivity, large one-time investment, etc., and achieves low production cost, low pollution and side effects. The effect of less product

Inactive Publication Date: 2011-05-25
ZHEJIANG XINHUA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The existing synthetic method has poor product selectivity, low target conversion rate, many by-products, serious equipment corrosion, large one-time investment, heavy pollution, and high production cost

Method used

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  • Synthesis method of N-methyl isopropylamine
  • Synthesis method of N-methyl isopropylamine
  • Synthesis method of N-methyl isopropylamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Preparation of 1,3,5-tri(isopropyl)hexahydro-1,3,5-triazine

[0015] In a 250ml four-necked flask equipped with a stirrer, a reflux condenser, a thermometer and a dropping funnel, add 60 g of anhydrous isopropylamine, use an ice-water bath to control the temperature at 5°C, stir rapidly, and add dropwise from the dropping funnel 35% formaldehyde solution 120g, in the case of rapid stirring, after 1h dripping, continue stirring in ice water bath for 4h, after the reaction is completed, the oil layer is separated, and dried with anhydrous magnesium sulfate for 12h to obtain 1,3,5-tris (Isopropyl) hexahydro-1,3,5-triazine is genuine product, with a content of 89.3% and a yield of 85.6%.

Embodiment 2-8

[0017] Preparation of 1,3,5-tri(isopropyl)hexahydro-1,3,5-triazine

[0018] The effect of reaction temperature on the reaction

[0019] The difference from Example 1 is that the reaction temperatures in Examples 2-4 are 1°C, 3°C, and 10°C, respectively. Other reaction conditions are the same as those in Example 1. The results are listed in Table 1 after chromatographic analysis.

[0020] Table 1 Influence of reaction temperature on reaction

[0021]

[0022] Table 2 Effects of different reaction conditions on the reaction

[0023]

Embodiment 9

[0025] Preparation of N-methylisopropylamine

[0026] 70g of zinc powder and 200ml of water were put into the three-necked flask, the temperature was controlled at -5°C, and 40g of 1,3,5-tris(isopropyl)hexahydro-1 was dropped simultaneously with a dropping funnel under strong stirring. 3,5-triazine and 320ml of concentrated hydrochloric acid are controlled to be dripped within 0.5h. After the dripping is completed, stirring is continued for 1h, and the remaining zinc powder is removed by filtration. Then 150ml of 40% sodium hydroxide solution was put into the three-necked flask of the reactive distillation unit, the temperature was controlled at 90°C, and the filtrate was slowly added dropwise with a dropping funnel under strong stirring, and the dropping was completed within 2 hours. Then continue to stir the reaction for 2h, and steam out the product N-methylisopropylamine while adding dropwise. Finally, after re-rectifying the N-methylisopropylamine obtained by reactive di...

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Abstract

The invention discloses a chemical synthesis method, particularly relates to a preparation method of synthesizing N-methyl isopropylamine by isopropamide. In the synthesis method, the N-methyl isopropylamine is prepared by a Mannich reaction and a decomposition reaction; in the first step, Mannich reaction of anhydrous isopropylamine and formalin solution is carried out; and in the step 2, the decomposition reaction is carried out as follows: respectively adding a reaction product 1,3,5-tri(isopropyl)hexhydro-1,3,5-triazine from the step 1 and concentrated hydrochloric acid in suspending liquid of znic powder and water at the same time, filtering to remove the residual zinc powder after reaction, then dropwise adding filtrate to aqueous sodium hydroxide solution for the decomposition reaction, steaming out the product N-methyl isopropylamine while dripping, and finally, refining, and then obtaining the N-methyl isopropylamine. The synthesis method has the advantages that the process flow is simple, the conversion rate is high, the selectivity is good, the byproducts are less, and the quality of product is stable.

Description

technical field [0001] The invention belongs to the synthetic field of organic chemical industry, and specifically refers to a preparation method of N-methyl isopropylamine. technical background [0002] N-methylisopropylamine (N-methylisopropylamine, CAS registration number 4747-21-1), also known as N-isopropyl methylamine, is liquid in appearance and has a boiling point of 50℃-53℃. It is an important pharmaceutical intermediate. , is the main raw material for the synthesis of pyramidone (which can be used as an antipyretic and analgesic). The existing synthesis method has poor product selectivity, low target conversion rate, many by-products, serious equipment corrosion, large one-time investment, large pollution and high production cost. SUMMARY OF THE INVENTION [0003] Aiming at the deficiencies existing in the prior art, the invention provides a synthetic method of N-methylisopropylamine with simple process and high yield. [0004] The present invention solves its ...

Claims

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Application Information

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IPC IPC(8): C07C211/08C07C209/62
Inventor 伍伟伟王卫明徐利红李道权谢自强陈宏
Owner ZHEJIANG XINHUA CHEM
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