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Microchannel reactor, and method for preparing N-alkoxyoxalyl alaninate by using microchannel reactor

A technology of alkoxy oxalylalanine ester and microchannel reactor, which is applied in chemical instruments and methods, chemical/physical/physicochemical reactors, carboxylic acid amide preparation, etc., which can solve the problem of low production efficiency and poor operation Complexity, low product yield, etc., to avoid product loss, simple post-processing, and shorten the reaction cycle

Active Publication Date: 2019-02-01
SHANDONG NHU FINE CHEM SCI & TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This reaction does not use toxic organic solvents such as benzene to carry water, and can realize continuous operation, but this method is based on the input of alanine, and the calculated product yield is not high; At the same time, the ethanol is continuously distilled, and the operation is complicated; and in order to obtain 900g of product, it needs to stay for more than 20 hours, and the production efficiency per unit time is not high

Method used

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  • Microchannel reactor, and method for preparing N-alkoxyoxalyl alaninate by using microchannel reactor
  • Microchannel reactor, and method for preparing N-alkoxyoxalyl alaninate by using microchannel reactor
  • Microchannel reactor, and method for preparing N-alkoxyoxalyl alaninate by using microchannel reactor

Examples

Experimental program
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Effect test

Embodiment 1

[0058] Put 400g of alanine, 651g of oxalic acid dihydrate, and 620g of ethanol into a 5L three-necked flask equipped with a stirring bar, a thermometer, and a condenser, and heat to dissolve at 80°C. After the heater is heated to 80-105°C, it is passed into the microchannel ceramic permeable membrane reactor for reaction. The cavity diameter of the membrane tube is 8mm, the flow rate of the feed liquid is 10ml / min, the pressure of the tube side is 0.3Mpa, and the pressure of the shell side is -0.1MPa. Dehydration while reacting, the reaction solution passing through the primary reactor enters the secondary and tertiary reactors for reaction, until the reaction system no longer has water detached and the reaction liquid water content is lower than 0.5%, the reaction is completed, and the total residence time is 20 hours; After finishing the reaction, the solvent in the reaction solution was removed by distillation under normal pressure, and diethyl oxalate was reclaimed by disti...

Embodiment 2

[0060] Put 400g of alanine, 651g of oxalic acid dihydrate, and 808g of n-propanol into a 5L three-necked flask equipped with a stirring bar, a thermometer, and a condenser, and heat to dissolve at 100°C. After the system is clarified, mix it evenly with 2346g of dipropyl oxalate , heated to 100-115°C by a heater, then passed into a microchannel ceramic permeable membrane reactor for reaction, the cavity diameter of the membrane tube is 8mm, the flow rate of the feed liquid is 10ml / min, the pressure of the tube side is 0.3Mpa, and the pressure of the shell side is -0.1 MPa, while dehydrating while reacting, the reaction liquid passing through the first-stage reactor enters the second and third-stage reactors to react until the reaction system no longer has water out and the water content of the reaction liquid is lower than 0.5%. The total residence time is 25%. hours; after finishing the reaction, the solvent in the reaction solution was removed by distillation under normal pre...

Embodiment 3

[0062] Put 400g of alanine, 651g of oxalic acid dihydrate, and 997g of n-butanol into a 5L three-necked flask equipped with a stirring bar, a thermometer, and a condenser, and heat to dissolve at 120°C. After the system is clarified, mix it evenly with 2723g of dibutyl oxalate , after being heated to 120-133°C by a heater, it is passed into a microchannel ceramic permeable membrane reactor for reaction. The cavity diameter of the membrane tube is 8mm, the flow rate of the feed liquid is 10ml / min, the pressure of the tube side is 0.3Mpa, and the pressure of the shell side is -0.1 MPa, while dehydrating while reacting, the reaction liquid passing through the first-stage reactor enters the second and third-stage reactors to react until the reaction system no longer has water out and the reaction liquid water content is lower than 0.5%. The total residence time is 28 hours; after finishing the reaction, the solvent in the reaction solution was removed by distillation at normal pres...

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Abstract

The invention discloses a microchannel reactor, and a method for preparing N-alkoxyoxalyl alaninate by using the microchannel reactor. The method comprises the following steps: a mixed solution of alanine, oxalic acid, C1-C8 alcohol and oxalic acid diester are introduced into the microchannel reactor and are reacted under a heating condition, water is removed by a permeable membrane during the reaction, and the obtained reaction solution is post-treated to obtain the N-alkoxyoxalyl alaninate. The method utilizes the internal microstructure and the excellent mass transfer and heat transfer capability of the microchannel reactor to realize efficient mass transfer of reaction materials and timely remove water generated by the reaction in order to promote the reaction, so the method has the advantage of high yield, low energy consumption, short cycle, good safety, environmental protection, and continuousness in operation.

Description

technical field [0001] The invention relates to a method for preparing N-alkoxy oxalyl alanine ester by using a microchannel reactor, and belongs to the technical field of organic chemical synthesis. Background technique [0002] N-alkoxy oxalyl alanine ester (structure shown in formula I) is a very important chemical intermediate, commonly used in the preparation of oxazoles, pyrazines, imidazoles and other compounds, especially widely used in vitamin The synthesis of B6 is a key intermediate in the synthesis of vitamin B6. [0003] [0004] R is a C1-C8 alkyl group. [0005] At present, the chemical synthesis method of N-alkoxy oxalyl alanine usually includes the following: [0006] (1) One-pot method: Simultaneous esterification and amidation reactions of alanine, alcohol and oxalic acid to synthesize the target product. According to relevant literature reports, alanine, industrial oxalic acid, and ethanol are mixed, and under the catalysis of hydrochloric acid, ben...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C233/56C07C231/02B01J19/00
CPCB01J19/0093C07C231/02C07C233/56Y02P20/141
Inventor 陈卫勇吴再红梁昊赵雷周岩童丽邵闪张志鹏雷超梁小雷张甲春陈洁
Owner SHANDONG NHU FINE CHEM SCI & TECH CO LTD
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