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Method for synthesizing N-isopropylbenzylamine

A technology of isopropylbenzylamine and isopropylamine, which is applied in the field of synthesis of N-isopropylbenzylamine, can solve the problems of many wastes, high cost, and high requirements for production equipment, and achieve good reaction selectivity, few by-products, The effect of high yield

Pending Publication Date: 2020-06-16
杭州益至生物科技有限公司
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AI Technical Summary

Problems solved by technology

The reducing agents used in the above two methods are mainly sodium borohydride and potassium borohydride, and these two reducing agents belong to the explosive chemicals clearly stipulated by the state. Within the scope of control, the production safety is poor, and there are It is a big safety hazard, and the post-treatment needs to be quenched with alkene acid, which produces more three wastes; other reducing agents include sodium triacetoxyborohydride, sodium cyanoborohydride, etc., but the cost is relatively high. Not suitable for large-scale industrial production
In addition to the above reduction method, you can also choose to add metal catalysts such as palladium carbon, Raney nickel, etc. to reduce by passing hydrogen under high pressure. However, this method has high requirements for production equipment, increased catalyst costs, and certain safety hazards when passing hydrogen.
Therefore, there are great difficulties in the source of N-isopropylbenzylamine

Method used

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  • Method for synthesizing N-isopropylbenzylamine

Examples

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Embodiment 1

[0020] (1) Ammonolysis reaction: put 71g of isopropylamine, 0.6g of copper oxide, and 120g of methanol into a 250ml reaction bottle, add 60g of benzyl chloride while stirring, react at 30°C until the reaction of the raw material benzyl chloride is complete, and cool the reaction solution to 0°C , filtered to remove the catalyst and the organic salts produced, and recovered methanol under reduced pressure to obtain the crude product of N-isopropylbenzylamine. , GC>99%.

Embodiment 2

[0022] (1) Ammonolysis reaction: drop 85g of isopropylamine, 1.2g of cuprous chloride, and 100g of ethanol into a 250ml reaction bottle, add 60g of benzyl chloride during stirring, react at 40°C until the reaction of the raw material benzyl chloride is complete, and cool the reaction solution to 0°C, remove the catalyst and the organic salt produced by filtration, recover ethanol under reduced pressure, and obtain the crude product of N-isopropylbenzylamine. %), GC>99%.

example 3

[0024] (1) Ammonolysis reaction: put 75g of isopropylamine, 6.0g of cuprous iodide, and 90g of ethyl acetate into a 250ml reaction bottle, add 60g of benzyl chloride while stirring, and react at 60°C until the reaction of the raw material benzyl chloride is complete. Cool down to 1°C, remove the catalyst and the generated organic salt by filtration, recover ethyl acetate under reduced pressure to obtain crude N-isopropylbenzylamine, and obtain 58.7g of pure N-isopropylbenzylamine after the crude product is rectified under reduced pressure (Yield 83.2%), GC>99%.

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Abstract

The invention provides a method for synthesizing N-isopropylbenzylamine, which comprises subjecting benzyl chloride as a raw material and isopropylamine to ammonolysis reaction under the action of a catalyst to obtain the N-isopropylbenzylamine. The process is simple in synthetic route, the reaction is easy to control, less three wastes are generated, and the green and environment-friendly requirements are met. The produced N-isopropylbenzylamine is high in purity and excellent in quality, and is an excellent industrialization route.

Description

technical field [0001] The invention relates to a synthesis method of N-isopropylbenzylamine. Background technique [0002] N-isopropylbenzylamine is an important pharmaceutical and chemical intermediate, and can be used as an additive for rust removers and joint pastes. [0003] There have been many studies on the preparation method of N-isopropylbenzylamine. At present, the preparation method of N-isopropylbenzylamine mainly uses benzaldehyde and isopropylamine as raw materials through reduction. The specific synthesis principle is that benzaldehyde and isopropylamine form a Schiff base, and then in an organic solvent, N-isopropylbenzylamine is obtained through reduction under the action of a reducing agent such as sodium borohydride. In addition to the above-mentioned methods, the known and reported preparation methods also include the reduction method of synthesizing a Schiff base reducing agent with benzylamine and acetone as raw materials. The reducing agents used in...

Claims

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Application Information

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IPC IPC(8): C07C209/08C07C211/27
CPCC07C209/08C07C211/27
Inventor 朱翼鸣倪燕霞
Owner 杭州益至生物科技有限公司
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