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Continuous synthesis method of 2-acetamido-5-nitroanisole

A technology for nitroanisole and o-anisole is applied in the field of continuous synthesis of 2-acetamido-5-nitroanisole, and can solve the problems of low product purity, poor product quality, low safety, and the like, To achieve the effect of improving the reaction rate, reducing the cost and easy operation

Active Publication Date: 2021-11-02
SHANDONG NORMAL UNIV EXPERIMENTAL PLANT CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] Aiming at the deficiencies of the prior art, the present invention provides a continuous synthesis method of 2-acetamido-5-nitroanisole from aspects such as production safety, production efficiency, product quality, economy, and environmental friendliness, and solves the problem of Problems such as complex operation in the production process, low safety, low product purity, poor product quality, and long time

Method used

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  • Continuous synthesis method of 2-acetamido-5-nitroanisole

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Embodiment 1

[0037] A kind of 2-acetamido-5-nitroanisole continuous synthetic method, carries out following steps successively:

[0038] (1) Pre-acylation: add 9000 g of acetic acid mixture with a mass fraction of 15% anthranil to the reaction kettle, and react at a temperature of 20°C for 1 hour;

[0039] (2) Amidation: Pump the acetic acid mixture reaction liquid and 859g acetic anhydride (8.8mol) into the first temperature zone of the microchannel reactor at the same time, mix and complete the amidation reaction; the first temperature zone is set 1 reaction module, the amidation temperature is 20°C, the residence time is 0.5min, and the amidation reaction solution is obtained;

[0040] (3) Nitration: Continue to flow the amidation reaction solution in step (2) to the second temperature zone of the microchannel reactor, and at the same time pump 728.5g 98% nitric acid (11.35mol) into the second temperature zone, mix and complete the nitration reaction, The second temperature zone is equ...

Embodiment 2

[0044] A kind of 2-acetamido-5-nitroanisole continuous synthetic method, carries out following steps successively:

[0045] (1) Pre-acylation: Add 9,000 g of acetic acid mixture with a mass fraction of 25% anthranil to the reactor, and heat up to 35°C for 5 hours;

[0046](2) Amidation: Pump the acetic acid mixture reaction liquid and 186.7g acetic anhydride (1.83mol) into the first temperature zone of the microchannel reactor at the same time, mix and complete the amidation reaction; the first temperature zone Set up 4 reaction modules, the amidation temperature is 35°C, the residence time is 2.0min, and the amidation reaction solution is obtained;

[0047] (3) Nitration: Continue to flow the amidation reaction solution in step (2) to the second temperature zone of the microchannel reactor, and pump 1529.4g 98% nitric acid (23.79mol) into the second temperature zone at the same time, mix and complete the nitration reaction, Set up 6 reaction modules in the second temperature...

Embodiment 3

[0051] A kind of 2-acetamido-5-nitroanisole continuous synthetic method, carries out following steps successively:

[0052] (1) Pre-acylation: Add 9,000 g of acetic acid mixture with a mass fraction of 20% anthranil to the reactor, and heat up to 30°C for 3 hours;

[0053] (2) Amidation: Pump the acetic acid mixture reaction liquid and 744.6g acetic anhydride (7.3mol) into the first temperature zone of the microchannel reactor at the same time, mix and complete the amidation reaction, the first temperature zone Set up 3 reaction modules, the amidation temperature is 30°C, and the residence time is 1.5min;

[0054] (3) Nitration: Continue to flow the amidation reaction solution in step (2) to the second temperature zone of the microchannel reactor, and at the same time pump 1126.3g 98% nitric acid (17.52mol) into the second temperature zone, mix and complete the nitration reaction, The second temperature zone is equipped with 4 reaction modules, the reaction temperature is 60°...

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Abstract

The invention mainly relates to the field of organic synthesis, and discloses a continuous synthesis process of 2-acetamido-5-nitroanisole. According to the process, a micro-channel continuous flow reactor is used as main reaction equipment, o-aminoanisole is used as a starting raw material, and continuous synthesis of 2-acetamido-5-nitroanisole is realized through pre-acylation, amidation and nitration. According to the process, a composite amidation reagent is adopted, so that the cost of raw materials is reduced, and the amidation reagent and a reaction solvent are unified; a continuous production process and equipment are introduced, so that continuous production is realized, the automation degree is improved, and the production safety risk is greatly reduced; and the reaction time, the generation of byproducts and the subsequent treatment difficulty are reduced, the nitration selectivity is improved, the win-win situation of economic benefits and environmental benefits is finally realized, and the development concept of green chemistry is met.

Description

technical field [0001] The invention relates to the field of chemical synthesis of dye intermediates, in particular to a continuous synthesis method of 2-acetylamino-5-nitroanisole. Background technique [0002] 2-Acetamido-5-nitroanisole is an intermediate for the preparation of red base B (2-amino-5-nitroanisole), which is an important organic dye, yellow or yellow-brown Powdery solid, mainly used for dyeing and printing of cotton fiber fabrics, and also used for the manufacture of organic pigments such as fast pigment, bordeaux, golden yellow, black, etc. It is widely used in the printing and dyeing industry, and has a large market demand. The synthetic method of red base B basically uses o-aminoanisole as a raw material, and is prepared in three steps of amidation, nitration and hydrolysis. The hydrolysis step is basically fixed at high temperature reflux with alkali or acid, so the intermediate 2-acetamido-5-nitrate The preparation of base anisole becomes the important...

Claims

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Application Information

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IPC IPC(8): C07C231/02C07C231/12C07C233/25B01J19/00
CPCC07C231/02C07C231/12B01J19/0093C07C233/25
Inventor 刘启奎杨松
Owner SHANDONG NORMAL UNIV EXPERIMENTAL PLANT CO LTD
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