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Method for preparing 6-nitroveratric acid from veratric acid in micro-channel reactor

A technology of microchannel reactor and nitroveratronic acid, which is applied in the field of medicine and chemical industry, can solve the problems of many ectopic nitration products, large amount of dilute nitric acid used, and low production efficiency, so as to improve yield and purity, and react Ease of exothermic control and short reaction time

Pending Publication Date: 2021-05-18
山东天铭医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] In view of the existing methods for preparing 6-nitroveratronic acid by nitration, there are large amounts of dilute nitric acid used, heat release is difficult to control, acid waste water is more, production efficiency is low, and there are many ectopic nitration products resulting in low product yield and low purity. Low-level problem, the invention provides a kind of method that microchannel reactor prepares 6-nitroveratronic acid by veratronic acid

Method used

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  • Method for preparing 6-nitroveratric acid from veratric acid in micro-channel reactor

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Effect test

Embodiment 1

[0028] Turn on the heating and preheating system of the microchannel reactor to raise the temperature of the system to the reaction temperature of 70°C. 1000g veratrol is dissolved in 2000g acetic acid, and the acetic acid solution of veratrol and 65% nitric acid are added in the microchannel reactor by meter, wherein flow rate: the acetic acid solution of veratrol is 30g / min, 65% nitric acid 6.38g / min, the reaction pressure is normal pressure.

[0029] The feed material stays in the microchannel reactor for 5 minutes, and the obtained acetic acid solution of 6-nitroveratronic acid is collected, including remaining concentrated nitric acid. The content of veratronic acid was detected by HPLC < 0.5%. The reaction solution was cooled to 15°C-20°C while stirring, filtered, washed with a small amount of water, and dried to obtain 1061g of 6-nitroveratronic acid with a yield of 85.1% and a purity of more than 99%.

Embodiment 2

[0031] Turn on the heating and preheating system of the microchannel reactor to raise the temperature of the system to the reaction temperature of 70°C. 1000g veratronic acid is dissolved in 2000g acetic acid, and the acetic acid solution of veratric acid and 65% nitric acid are joined in the microchannel reactor by meter, wherein flow velocity is the acetic acid solution 30g / min of veratronic acid, 65% nitric acid 10.6 g / min, and the reaction pressure is normal pressure.

[0032] The feed material stays in the microchannel reactor for 5 minutes, and the obtained acetic acid solution of 6-nitroveratronic acid is collected, including remaining concentrated nitric acid. Veratronic acid was detected by HPLC < 0.2%. The reaction solution was stirred and lowered to 15°C-20°C, filtered, washed with a small amount of water, and dried to obtain 1080g of 6-nitroveratronic acid with a yield of 86.7% and a purity of more than 99%.

Embodiment 3

[0034] Turn on the heating and preheating system of the microchannel reactor to raise the temperature of the system to the reaction temperature of 80°C. 1000g veratronic acid is dissolved in 2000g acetic acid, and the acetic acid solution of veratric acid and 65% nitric acid are joined in the microchannel reactor by meter, wherein flow rate is the acetic acid solution 30g / min of veratronic acid, 65% nitric acid 6.38 g / min, the reaction pressure is 1MPa.

[0035] The feed material stays in the microchannel reactor for 5 minutes, and the obtained acetic acid solution of 6-nitroveratronic acid is collected, including remaining concentrated nitric acid. Veratronic acid was detected by HPLC < 0.5%. The reaction liquid was stirred and lowered to 15°C-20°C, filtered, washed with a small amount of water, and dried to obtain 1069g of 6-nitroveratronic acid with a yield of 85.8% and a purity of more than 99%.

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Abstract

The invention provides a method for preparing 6-nitroveratric acid from veratric acid through a micro-channel reactor, aiming at solving the problems of low product yield, low purity and the like caused by large dilute nitric acid usage amount, difficulty in heat release control, much acidic wastewater, low production efficiency and more reaction ectopic nitration products in the existing method for preparing 6-nitroveratric acid through nitration. The invention provides the method for preparing 6-nitroveratric acid from veratric acid through the micro-channel reactor. According to the method, acetic acid is used as a solvent, veratric acid and concentrated nitric acid are used as raw materials, the reaction is performed in the micro-channel reactor, continuous production is realized, reaction heat release is easy to control, the production period is greatly shortened, the yield of 6-nitroveratric acid can reach 85% or above, and the purity of 6-nitroveratric acid can reach 99% or above.

Description

technical field [0001] The invention belongs to the field of medicine and chemical industry, and relates to a method for preparing 6-nitroveratronic acid from veratronic acid in a microchannel reactor. Background technique [0002] 6-Nitroveratronic acid is an important pharmaceutical intermediate and chemical raw material, mainly used as a pharmaceutical intermediate for the synthesis of quinazoline drugs (CN201910962926.1, CN201510279335.6, CN201510279465.X). 6-nitroveratronic acid, chemical name: 4,5-dimethoxy-2-nitrobenzoic acid, its molecular formula: C 9 h 8 NO 6 , the structural formula is as follows: [0003] [0004] The synthetic method of existing 6-nitroveratronic acid is generally obtained by reacting veratronic acid and dilute nitric acid under heating conditions, and the reaction equation is as follows: [0005] [0006] This method needs to use more dilute nitric acid (more than 5 times the molar amount), and there are many acidic wastewaters in the...

Claims

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Application Information

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IPC IPC(8): C07C201/08C07C205/59B01J19/00
CPCC07C201/08B01J19/0093C07C205/59
Inventor 宁尚恩周键孙崇国邢杨杨李松松朱玉正
Owner 山东天铭医药科技有限公司
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