Unlock instant, AI-driven research and patent intelligence for your innovation.

A kind of synthesis process of n,n-dimethylglycine sodium salt suitable for large-scale production

A technology of sodium dimethyl glycinate and synthesis process, which is applied in the preparation of organic compounds, organic chemistry, chemical instruments and methods, etc., to achieve the effects of simple process, convenient operation and cost reduction

Active Publication Date: 2015-09-02
山东祥维斯生物科技股份有限公司
View PDF0 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved by the present invention is to provide a synthesis process of N,N-dimethylglycine sodium salt suitable for large-scale production, the synthesis route is simple and clear, the yield is high, and no pollutants are produced, thereby eliminating the above-mentioned background technology Medium defect

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Weigh 2000mol of chloroacetic acid and place in the reaction kettle of 1000L, add n-butanol 3000mol, 12kg of p-toluenesulfonic acid successively, stir mechanically, be warming up to 60 ℃, reflux and divide water; Weigh 4000mol of dimethylamine and place the reaction of 2000L In the kettle, the reaction solution of the previous step was added at 60 °C, and the temperature was controlled to 60 °C. After the dropwise addition was completed, the temperature was kept for 1.0 h; the organic phase of the reaction solution of the previous step was separated, and 120 kg of n-butanol was added to the aqueous phase for extraction , combine the organic phases; concentrate the organic phase in vacuo to recover n-butanol; heat the remaining organic phase to 80 ° C, add liquid alkali to adjust the pH to 7, keep the temperature at this temperature for 2 h, cool down, filter and dry to obtain 213.74 kg of product, the yield is 213.74 kg. was 85.49%.

[0027] Indicator name

Embodiment 2

[0029] Take by weighing 4000mol of chloroacetic acid and place in the reactor of 2000L, add 6000mol of n-butanol, 20kg of p-toluenesulfonic acid, stir mechanically, be warming up to 66 ℃, reflux and separate water; take by weighing 8000mol of dimethylamine and place in the reactor of 4000L , add the reaction solution of the previous step at 53 ° C, control the temperature to 53 ° C, and keep the temperature at this temperature for 1.5 h after the dropwise addition; separate the organic phase of the reaction solution of the previous step, add 249 kg of n-butanol to the aqueous phase for extraction, and combine Organic phase; vacuum-concentrated the organic phase to recover n-butanol; heat the remaining organic phase to 70°C, add liquid caustic soda to adjust pH to 9, keep the temperature at this temperature for 2.5h, cool down, filter, and dry to obtain 405.18kg of product with a yield of 405.18kg. 81.03%.

[0030] Indicator name

[0031] Arsenic (as As), mg / ...

Embodiment 3

[0033] Take by weighing 6000mol of chloroacetic acid and place in the reactor of 4000L, add 9000mol of n-butanol, 42kg of p-toluenesulfonic acid, stir mechanically, be warming up to 70 ℃, reflux and separate water; take by weighing 12000mol of dimethylamine and place in the reactor of 6000L , add the reaction solution of the previous step at 50 °C, control the temperature to 50 °C, and keep the temperature at this temperature for 2 h after the dropwise addition; separate the organic phase of the reaction solution of the previous step, add 374 kg of n-butanol to the aqueous phase for extraction, and combine the organic Concentrate the organic phase in vacuo to recover n-butanol; heat the remaining organic phase to 87°C, add liquid alkali to adjust the pH to 8.6, keep the temperature at this temperature for 3h, cool down, filter, and dry to obtain 628.31kg of product with a yield of 83.77% .

[0034] Indicator name

N,N-Dimethylglycine sodium salt

color

W...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
densityaaaaaaaaaa
flash pointaaaaaaaaaa
Login to View More

Abstract

A synthesis process of N,N-dimethylglycine sodium salt suitable for large-scale production, comprising the following steps: weighing chloroacetic acid and placing it in a reaction kettle, adding n-butanol and p-toluenesulfonic acid in sequence, stirring mechanically, and raising the temperature to 60°C~70°C, reflux to separate water; weigh dimethylamine and place it in a reaction kettle, add the reaction solution at 50°C~60°C, after the addition is completed, keep it warm at this temperature for 1h~2h; The organic phase of the reaction solution is obtained, the water phase is extracted by adding n-butanol, and the organic phases are combined; the obtained organic phase is concentrated in vacuum, and n-butanol is recovered; Adjust the pH to 7-9, keep warm at this temperature for 2h-3h, cool down, filter, and dry to obtain the product. The synthetic preparation process provided by the invention has easy-to-obtain and cheap raw materials, simple process, convenient operation, no difficulty in purification, low cost, and no discharge of "three wastes".

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a synthesis process of N,N-dimethylglycine sodium salt suitable for large-scale production. Background technique [0002] At present, N,N-Dimethylglycine sodium salt, English name: N,N-Dimethylglycinesodium salt CAS number: 18319-88-5, molecular weight: 127.11, molecular formula: C 4 H 8 NNaO 2 , density: 1.069g / cm3, boiling point: 175.2 ℃ at760mmHg, flash point: 59.8 ℃, white flaky crystal or powder. [0003] N,N-Dimethylglycine sodium salt is an endogenous compound sodium salt, and it is also a very effective metabolic enzyme in vivo. Because of its amphiphilic molecular structure, it has many unique functions and can stimulate B cells produce higher antibody responses and enhance the activity of T cells and macrophages, so as a drug N,N-dimethylglycine sodium salt can be used to treat depression, improve human immunity, and enhance human tolerance. In addition, ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07C229/12C07C227/18
Inventor 马兴群丁振柱曾凡伟张守伟张毅丰孟涛
Owner 山东祥维斯生物科技股份有限公司