Preparation method of N, N-dimethylglycine for industrial production

A technology of dimethylglycine and dimethylamine, which is applied in the field of preparation of pharmaceutical chemical intermediates, can solve the problems of reduced yield, difficult to obtain, serious environmental pollution and the like, and achieves the effects of stable preparation method, convenient operation and simple process

Active Publication Date: 2013-12-25
山东祥维斯生物科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 2. Formaldehyde reacts with glycine to prepare N,N-dimethylglycine in formic acid environment. This method is not easy to obtain pure N,N from formic acid system. Dimethylglycine;
[0006] 3. Using glycine and formaldehyde as raw materials in the presence of palladium/carbon catalyst to synthesize N,N by hydrogenation under normal pressure. Dimethylglycine, the catalyst for this method is too expensive;
[0007] 4. Dimethylamine reacts with hydroxyacetonitrile, and then hydrolyzes to obtain N,N-dimethylglycine. This method also uses cyanide, which seriously pollutes the environment;
[0008] 5. Chloroacetic acid reacts with sodium hydroxide to generate sodium chloroacetate, and sodium chloroacetate reacts with dimethylamine. After...

Method used

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Effect test

Embodiment 1

[0025] A preparation method suitable for industrialized production of N,N-dimethylglycine, comprising the steps of:

[0026] S1, preparation of chloroacetic acid solution: at normal temperature, 100kg of chloroacetic acid was added to 100kg of water to obtain a chloroacetic acid solution;

[0027] S2. Reaction with dimethylamine: add the chloroacetic acid solution to 416kg of 40wt% dimethylamine aqueous solution, and control the temperature to 20°C, and keep the reaction for 2 hours after completion;

[0028] S3. Removal of excess dimethylamine: after the reaction is completed, remove unreacted dimethylamine. When removing excess dimethylamine, the temperature is controlled at 90° C., and the pH at the end point is controlled to be 6.4;

[0029] S4. Concentrate crystallization, centrifuge, and dry: Concentrate the above solution until a large amount of white crystals appear, lower the temperature to 25° C., centrifuge, and dry. The concentration temperature is controlled at 9...

Embodiment 2

[0032] A preparation method suitable for industrialized production of N,N-dimethylglycine, comprising the steps of:

[0033] S1, preparation of chloroacetic acid solution: at normal temperature, 120kg of chloroacetic acid was added to 120kg of water to obtain a chloroacetic acid solution;

[0034] S2. Reaction with dimethylamine: adding chloroacetic acid solution to 430kg of 40wt% dimethylamine aqueous solution, and controlling the temperature to 40°C, and keeping it warm for 3 hours after completion;

[0035] S3. Removal of excess dimethylamine: after the reaction is completed, remove unreacted dimethylamine. When removing excess dimethylamine, the temperature is controlled at 95° C., and the pH at the end point is controlled to be 6.0;

[0036] S4 concentrated crystallization, centrifugation, and drying: Concentrate the above solution until a large amount of white crystals appear, lower the temperature to 25° C., centrifuge, and dry. The concentration temperature is control...

Embodiment 3

[0039] A preparation method suitable for industrialized production of N,N-dimethylglycine, comprising the steps of:

[0040] S1, preparation of chloroacetic acid solution: at normal temperature, 125kg of chloroacetic acid was added to 125kg of water to obtain a chloroacetic acid solution;

[0041] S2. Reaction with dimethylamine: add the chloroacetic acid solution to 596kg of 40wt% dimethylamine aqueous solution, and control the temperature to 50°C, and keep the reaction for 4 hours after completion;

[0042] S3. Removal of redundant dimethylamine: after the reaction is completed, remove unreacted dimethylamine, and control the temperature at 100°C when removing redundant dimethylamine, and control the end point pH to 5.5;

[0043] S4 concentrated crystallization, centrifugation, and drying: Concentrate the above solution until a large amount of white crystals appear, lower the temperature to 25° C., centrifuge, and dry. The concentration temperature is controlled at 105°C, t...

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Abstract

The invention discloses a preparation method of N, N-dimethylglycine for industrial production. The preparation method comprises the following steps of S1, chloroacetic acid solution preparation: adding chloroacetic acid into water at a normal temperature to obtain a chloroacetic acid solution, S2, reaction of the chloroacetic acid solution and dimethylamine: adding the chloroacetic acid solution into a dimethylamine agueous solution according to a more ratio of chloroacetic acid to dimethylamine of 1: 2.5 to 1: 5, controlling a temperature in 20-70 DEG C, and then carrying out a thermal insulation reaction process at the temperature of 20-70 DEG C for 2-5h, S3, redundant dimethylamine removal: removing unreacted dimethylamine after the thermal insulation reaction, and S4, condensation crystallization, centrifugation and drying: concentrating the solution obtained by the step S3 to obtain a lot of white crystals, carrying out cooling to a temperature of 25 DEG C, and carrying out centrifugation and drying. The preparation method adopts the easily-available and cheap raw materials, has simple processes, is convenient for operation, has no purification difficulty and is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to a preparation method of a pharmaceutical chemical intermediate, in particular to a preparation method of N,N-dimethylglycine suitable for industrial production. Background technique [0002] At present, N,N-dimethylglycine can be used as a drug to treat depression, improve human immunity, and enhance human tolerance. The methyl group in the structure has the function of transmethylation, which can be used to resist tumors and cancers, and can be widely used in the synthesis of anticancer drugs. N,N-Dimethylglycine can be used as a skin penetration enhancer and cosmetic additive due to its strong water absorption. At the same time, the antioxidant and non-toxic properties of N,N-dimethylglycine can be used as an antioxidant in food. [0003] The methods for preparing N,N-dimethylglycine in the past include: [0004] 1. Prepare N,N-dimethylglycine by reacting sodium cyanide, dimethylamine, sodium bisulfite and formaldehyde. Th...

Claims

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Application Information

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IPC IPC(8): C07C229/12C07C227/08
Inventor 马兴群张守伟丁振柱张毅丰曾凡伟
Owner 山东祥维斯生物科技股份有限公司
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