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Preparation method of 3-(N,N-diallyl)amino-4-methoxy acetanilide

A technology of methoxyacetanilide and diallyl is applied in the field of continuous preparation of 3-amino-4-methoxyacetanilide by using a microreactor, which can solve the problems of long reaction time and low production efficiency, and achieves the The effect of shortening reaction time, improving production efficiency and high yield

Active Publication Date: 2019-07-05
ZHEJIANG LONGSHENG CHEM RES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 3-(N,N-diallyl)amino-4-methoxyacetanilide is usually 2-amino-4-acetamidoanisole reacted with allyl chloride for more than 10 hours under the condition of acid-binding agent, even The organic solvent and catalyst are added in the reaction, and the reaction time is more than 5 hours. The existing technology has problems such as long reaction time and low production efficiency.

Method used

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  • Preparation method of 3-(N,N-diallyl)amino-4-methoxy acetanilide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Please refer to figure 1, the invention provides a reaction device for preparing 3-(N,N-diallyl)amino-4-methoxyacetanilide, comprising two feed tanks (1 is feed tank A, and the material contained in it is A includes 2-amino-4-acetamidoanisole, acid-binding agent and water, 3 is feed tank B, the material B in it includes allyl chloride), high-temperature pump A (2), pump B (4), T Type mixer (5), oil bath (6), spiral tubular microreactor (7, 316L stainless steel material with an inner diameter of 0.5mm), back pressure valve (8), discharge tank (9), 4 with Insulated pipelines (10-13), 2 uninsulated pipelines (14 and 15). The feed tank A (1) is connected to the high-temperature pump A (2) through a pipeline (10) with insulation, and the high-temperature pump A (2) is connected to the T-type mixer (5) through a pipeline (11) with insulation; Tank B (3) is connected to pump B (4) through pipeline (14), and pump B (4) is connected to T-type mixer (5) through pipeline (15); t...

Embodiment 2

[0043] Reactor see figure 1 , Mix 2-amino-4-acetamidoanisole, water, and sodium acetate at a mass ratio of 1:19:1.9, heat up to 90°C as material A; chloropropene as material B. Material A and material B are continuously entered into the helical tubular microreactor (7, the inner diameter of the pipe is 0.5mm) through the T-type mixer (5) at 1.46g / min and 0.11g / min speed respectively, and passed through the oil bath (6 ) to control the reaction temperature to 120°C, the back pressure valve (8) to control the reaction pressure to 1.0Mpa, and the reaction residence time to be 12min. The product of 4-methoxyacetanilide has a purity of 89.81% and a yield of 94.1%.

Embodiment 3

[0045] Reactor see figure 1 , mix 2-amino-4-acetamidoanisole, water, sodium acetate and dimethylacetamide at a mass ratio of 1:8:1.7:1, heat up to 90°C as material A; mix allyl chloride and ethanol with Mass ratio 1:2.3 mixed, as material B. Material A and material B are continuously entered into the helical tubular microreactor (7, the inner diameter of the pipe is 0.5mm) through the T-type mixer (5) at 0.52g / min and 0.28g / min speed respectively, and passed through the oil bath (6 ) to control the reaction temperature to 120°C, the back pressure valve (8) to control the reaction pressure to 1.0Mpa, and the reaction residence time to be 10min. - Methoxyacetanilide product, purity 91.81%, yield 95%.

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Abstract

The invention discloses a preparation method of 3-(N,N-diallyl)amino-4-methoxy acetanilide. The preparation method comprises the following steps: (1) respectively preparing a material A and a materialB, and heating the material A to 60-100 DEG C, wherein the material A comprises 2-amino-4-acetamidoanisole, water and an acid-binding agent, and the material B comprises chloropropene; (2) separatelyand continuously feeding the material A and the material B into a micro-reactor, controlling the mixing mass ratio of the 2-amino-4-acetamidoanisole to the chloropropene to be 1:(0.8-5.0), and carrying out a reaction at 80-180 DEG C under pressure of 0.4-40 MPa, wherein the micro-reactor is a tubular micro-reactor, the inner diameter of a tube is 0.4-1.6 mm, the micro-reactor is made of meltablepolytetrafluoroethylene, polyether-ether-ketone or 316L stainless steel; and (3) separating the materials obtained from the reaction to obtain a target product. According to the method disclosed by the invention, the micro-reactor is used for realizing continuous preparation of the 3-(N,N-diallyl)amino-4-methoxy acetanilide, the reaction time can be remarkably shortened, and the obtained product is high in yield and high in purity.

Description

[0001] (1) Technical field [0002] The invention relates to a preparation method of 3-(N,N-diallyl)amino-4-methoxyacetanilide, in particular to a method for continuously preparing 3-(N,N-diene Propyl)amino-4-methoxyacetanilide method. [0003] (2) Background technology [0004] 3-(N,N-diallyl)amino-4-methoxyacetanilide is an important intermediate for the synthesis of disperse blue 291:1, and disperse blue 291:1 has been widely promoted and used in recent ten years. Dye, excellent dyeing effect on polyester, bright color after dyeing, excellent wash fastness. Disperse Blue 291:1 can be used instead of Disperse Blue 291 without affecting the dyeing effect. Disperse Blue 291:1 can be used alone or combined. It can be combined to produce Disperse Dark Blue RD-2R and Disperse Black EX-SF with excellent quality and low cost, increasing the variety of products. [0005] 3-(N,N-diallyl)amino-4-methoxyacetanilide is usually 2-amino-4-acetamidoanisole reacted with allyl chloride for...

Claims

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Application Information

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IPC IPC(8): C07C233/43C07C231/12
CPCC07C231/12C07C233/43
Inventor 何旭斌荆钰孟福庆张淼陈晓晓邱雯
Owner ZHEJIANG LONGSHENG CHEM RES
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