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Method for producing bi(2-hydroxyethyl)imino-tri(hydroxymethyl)methyl hydride

A technology of trishydroxymethylaminomethane and iminotrimethane, which is applied in the field of preparing diiminotrimethane, can solve the problems of combustion and explosion, ethylene oxide is explosive and flammable, and requires high equipment, and achieves low cost and low raw material consumption. , equipment requires simple effect

Inactive Publication Date: 2011-03-23
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In foreign countries, trishydroxymethylaminomethane and ethylene oxide are used as raw materials to prepare this product, but this method requires high equipment, and ethylene oxide is explosive and flammable, and it can cause combustion and explosion if the concentration in the air exceeds 3%.

Method used

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  • Method for producing bi(2-hydroxyethyl)imino-tri(hydroxymethyl)methyl hydride
  • Method for producing bi(2-hydroxyethyl)imino-tri(hydroxymethyl)methyl hydride

Examples

Experimental program
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Effect test

Embodiment 1

[0011] Add 24g (0.2mol) of trishydroxymethylaminomethane, 16g of water, and 35g of chloroethanol into a three-necked flask equipped with a condenser, and stir and react at a temperature of 60° C. for 4 hours, then the reaction system is cooled to room temperature. At room temperature, slowly add 52g NaOH aqueous solution (concentration is about 5mol / L) dropwise, after adding, react at 60°C for 4 hours, cool to room temperature, slowly add 52g NaOH aqueous solution (concentration is about 5mol / L), and then The reaction was incubated at 60° C. for 60 hours.

[0012] Heat under reduced pressure to distill off the water, add 112ml of ethanol, heat to dissolve the viscous liquid completely, filter to remove NaCl, distill the filtrate to remove ethanol under reduced pressure, add 118g of n-butanol to the oily viscous liquid, and dissolve the viscous liquid under heating , After cooling, a solid precipitated out, and it was filtered under reduced pressure, the solid was washed with e...

Embodiment 2

[0014] Add 24g (0.2mol) of trishydroxymethylaminomethane, 16g of water, and 38g of chloroethanol into a three-necked flask equipped with a condenser, stir and react at a temperature of 60° C. for 4 hours, and then the reaction system is cooled to room temperature. At room temperature, slowly add 52g NaOH aqueous solution (concentration is about 5mol / L) dropwise. After completion, the reaction was incubated at 60° C. for 60 hours.

[0015] Heat under reduced pressure to distill off the water, add 112ml of ethanol, heat to dissolve the viscous liquid completely, filter to remove NaCl, distill the filtrate to remove ethanol under reduced pressure, add 118g of n-butanol to the oily viscous liquid, and dissolve the viscous liquid under heating , After cooling, a solid precipitated out, and it was filtered under reduced pressure, the solid was washed with ethyl acetate, and then dried in vacuo to obtain the product. The n-butanol mother liquor is evaporated to remove the n-butanol ...

Embodiment 3

[0017] Add 24g (0.2mol) of trishydroxymethylaminomethane, 16g of water, and 41.5g of chloroethanol into a three-necked flask equipped with a condenser, stir and react at a temperature of 60°C for 4 hours, and then the reaction system is cooled to room temperature. At room temperature, slowly add 52g NaOH aqueous solution (concentration is about 5mol / L) dropwise. After completion, the reaction was incubated at 60° C. for 60 hours.

[0018] Heat under reduced pressure to distill off the water, add 112ml of ethanol, heat to dissolve the viscous liquid completely, filter to remove NaCl, distill the filtrate to remove ethanol under reduced pressure, add 118g of n-butanol to the oily viscous liquid, and dissolve the viscous liquid under heating , After cooling, a solid precipitated out, and it was filtered under reduced pressure, the solid was washed with ethyl acetate, and then dried in vacuo to obtain the product. The n-butanol mother liquor is evaporated to remove the n-butanol ...

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Abstract

The invention discloses a method for preparing di (2-ethoxyl) imino-tri (hydroxymethyl) methane. The method comprises the following steps: using trihydroxymethylaminomethane and ethylene chlorohydrin as raw materials, adding water to be mixed and stirred, controlling a temperature at 60 DEG C, reacting for 4 hours, reducing the reaction system to room temperature, dropping an NaOH solution, heating up to 60 DEG C after finishing dropping, reacting for 4 hours, reducing to the room temperature again, dropping the NaOH solution, heating up to 60 DEG C after finishing dropping, and continuously reacting for 60 hours. The molar ratio of the trihydroxymethylaminomethane to the ethylene chlorohydrin is 1 to 2.2-2.6. After the reaction is finished, the mixture is heated under reduced pressure tovaporize water, and then extracted by anhydrous ethyl alcohol and recrystallized by n-butanol, so as to obtain the product di (2-ethoxyl) imino-tri (hydroxymethyl) methane. The method has the advantages of simple equipment requirements, raw material conservation, low cost and high efficiency, is suitable for industrial production, and obtains a product the yield of which is more than 90 percent and the purity of which is more than 99 percent.

Description

technical field [0001] The present invention relates to a process for the preparation of bis(2-hydroxyethyl)iminotris(hydroxymethyl)methane. Background technique [0002] Bis(2-hydroxyethyl)iminotris(hydroxymethyl)methane is an amphoteric buffer reagent, which is widely used in the research of biochemistry and molecular biology. It can provide a buffer pH range of 6.15-8.35 between. As a biological buffer, it is mainly used in biochemical diagnostic reagents, DNA / RNA extraction reagents and PCR diagnostic kits. [0003] There is no domestic report on the preparation of bis(2-hydroxyethyl)iminotris(hydroxymethyl)methane. In foreign countries, trishydroxymethylaminomethane and ethylene oxide are used as raw materials to prepare the product, but this method requires high equipment, and ethylene oxide is explosive and flammable, and its concentration in the air exceeds 3%, which can cause combustion and explosion. Contents of the invention [0004] The object of the present...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C215/12C07C213/00
Inventor 余明新乐优凤方海燕康君辉刘玲秀
Owner ZHEJIANG UNIV