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Piping production process of N-(2-hydroxyethyl)-beta-D-pyran glucosamine

A technology for glucopyranosamine and glucopyranose, which is applied in the field of preparing N--β-D-glucopyranosamine by using a pipeline reactor, can solve the problem of N-(2-hydroxyethyl)- The preparation process conditions and purification method of β-D-glucopyranosamine, the separation and purification method of N-(2-hydroxyethyl)-β-D-glucopyranosamine, and the strict requirements of process conditions are not involved, so as to achieve high purity , good color and high reaction temperature

Inactive Publication Date: 2008-10-15
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In 2005, Chinese patent CN 1611485A and in 2007, Chinese patent CN 1962610A disclosed the method of directly obtaining analogue N-(2-hydroxyethyl)-glucosamine by one-step method of catalytic hydrogenation, but did not specifically mention N-(2- Preparation process conditions and purification method of hydroxyethyl)-β-D-glucopyranosesamine
[0005] And the patent CN 1063754C once disclosed a kind of method for preparing N-alkyl polyhydroxyl alkylamine in aqueous / hydroxyl solvent, which relates to the method for preparing the intermediate product in a tank reactor; Reactor, which is a batch operation, and the reaction has strict requirements on process conditions. If the reactant stays at a higher temperature for too long, the color of the product will be darker, and the by-products will increase, which will affect the product quality; if the reaction time is too short, The raw material conversion rate is low
Therefore, the reaction technology needs to be improved
[0006] In addition, none of the above patents involves the separation and purification method of N-(2-hydroxyethyl)-β-D-glucopyranosesamine

Method used

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  • Piping production process of N-(2-hydroxyethyl)-beta-D-pyran glucosamine
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  • Piping production process of N-(2-hydroxyethyl)-beta-D-pyran glucosamine

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Embodiment 1

[0020] Embodiment 1, Fig. 1 have provided a kind of pipeline reactor, comprise raw material tank 1, metering pump 4, pipeline reactor 14 and condenser 11; The top of raw material tank 1 is provided with feed pipe 15 and discharge pipe 17 respectively , The feed pipe 15 is provided with a shut-off valve IV16, and the exhaust pipe 17 is provided with a shut-off valve V 18. The bottom outlet of the raw material tank 1 is connected with the metering pump 4 through the pipeline I3, and the metering pump 4 is connected with the inlet of the pipeline reactor 14 through the pipeline II5, and the outlet of the pipeline reactor 14 is connected with the inlet of the condenser 11 through the pipeline III9 Connected, the outlet of condenser 11 is connected with pipeline IV13. A cut-off valve I 2 is arranged on the pipeline I 3, a pressure gauge I 6 and a shut-off valve II 7 are respectively arranged on the pipeline II 5 according to the liquid flow direction, a thermometer 8 is arranged on...

Embodiment 2

[0023] Embodiment 2, a method for pipelined production of N-(2-hydroxyethyl)-β-D-glucopyranosesamine, adopts the pipeline reactor described in Example 1, and performs the following steps in sequence:

[0024] 1), raw material preparation:

[0025] Add glucose monohydrate 33g (0.17mol) in raw material tank 1, the solvent that each 50ml of methanol and water are formed; Shake well, glucose monohydrate is fully dissolved; Then add ethanolamine 13ml (0.20mol), shake well; Obtain mixing liquid.

[0026] 2), amination reaction:

[0027] Use the metering pump 4 to inject the above-mentioned mixed solution into the pipeline reactor 14, the reaction temperature is 60°C, and the reaction pressure is normal pressure; The reaction time is 140ml / h, that is, the reaction time is about 20mins. Follow up the reaction with TLC, the glucose point disappears, and the reaction ends, and the crude product solution containing N-(2-hydroxyethyl)-β-D-glucopyranosesamine.

[0028] 3), post-processi...

Embodiment 3

[0030] Embodiment 3, a method for pipelined production of N-(2-hydroxyethyl)-β-D-glucopyranosesamine, adopts the pipeline reactor described in Example 1, and performs the following steps in sequence:

[0031] 1), raw material preparation:

[0032] Add anhydrous glucose 30g (0.17mol) in raw material tank 1, the solvent that methanol 60ml and water 50ml form; Shake up, make anhydrous glucose fully dissolve; Then add ethanolamine 13ml (0.20mol), shake up; Obtain mixing liquid.

[0033] 2), amination reaction:

[0034] Use the metering pump 4 to inject the above-mentioned mixed solution into the pipeline reactor 14, the reaction temperature is 70°C, and the reaction pressure is 1.0Mpa; The reaction time is 180ml / h, that is, the reaction time is about 15mins, and the reaction is tracked by TLC. The glucose point disappears, and the reaction is ended, and the crude product solution containing N-(2-hydroxyethyl)-β-D-glucopyranosesamine is obtained.

[0035] 3), post-processing:

...

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Abstract

The invention discloses a method for realizing pipeline production of N-(2-ethoxyl)-Beta-D-glucopyranosylamine. The method is as follows: ethanolamine and glucose at the molar ratio of between 1:1 and 5:1 are used as a raw material which is mixed with solvent to obtain a mixed solution; the mixed solution is pumped into a pipeline reactor by a metering pump to carry out amination reaction, thereby obtaining a crude product solution containing N-(2-ethoxyl)-Beta-D-glucopyranosylamine under a pressure of between normal pressure and 2.0 MPa, at the temperature of between 40 and 80 DEG C for 10 to 30 mins. The method adopted to manufacture N-(2-ethoxyl)-Beta-D-glucopyranosylamine can obtain high rate of conversion at less energy consumption.

Description

technical field [0001] The invention relates to a chemical synthesis method, in particular to a method for preparing N-(2-hydroxyethyl)-β-D-glucopyranosesamine using a pipeline reactor. Background technique [0002] N-(2-hydroxyethyl)-β-D-glucopyranosesamine is an important intermediate of the antidiabetic drug Miglitol, and its structural formula is: [0003] [0004] In 2005, Chinese patent CN 1611485A and in 2007, Chinese patent CN 1962610A disclosed the method of directly obtaining analogue N-(2-hydroxyethyl)-glucosamine by one-step method of catalytic hydrogenation, but did not specifically mention N-(2- Hydroxyethyl)-β-D-glucopyranosesamine preparation process conditions and purification methods. [0005] And the patent CN 1063754C once disclosed a kind of method for preparing N-alkyl polyhydroxyl alkylamine in aqueous / hydroxyl solvent, which relates to the method for preparing the intermediate product in a tank reactor; Reactor, which is a batch operation, and th...

Claims

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Application Information

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IPC IPC(8): C07H15/12B01J19/24
Inventor 陈新志王帅陈小祥张旭
Owner ZHEJIANG UNIV
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