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Preparation method of 1, 3-bis (tri (hydroxymethyl) methylamino) propane

A technology of methylamino and hydroxymethyl, which is applied in the field of preparation of 1,3-bismethylamino)propane, can solve problems such as hindering large-scale application, low yield, and low purity, and achieve easy purification and separation, and product purity High, high-purity effect

Active Publication Date: 2022-06-07
SUZHOU YACOO SCI CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But in general, especially the number of patents in 1,3-bis(tris(hydroxymethyl)methylamino)propane is relatively small. Among the existing patents, there are still many problems in the preparation process, such as: Low yield, low purity and other issues
If the above problems are not solved, it will hinder their large-scale application, especially hindering their becoming a material in the field of biological buffers.

Method used

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  • Preparation method of 1, 3-bis (tri (hydroxymethyl) methylamino) propane
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  • Preparation method of 1, 3-bis (tri (hydroxymethyl) methylamino) propane

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Embodiment 1

[0040] A preparation method of 1,3-bis(tri(hydroxymethyl)methylamino)propane, comprising the following preparation steps:

[0041] Preparation step S1:

[0042]

[0043] Under stirring conditions, add 100 g of 3-chloropropanol to a 1 L dry reactor, the reaction temperature is 200 ° C, the reaction pressure is 1 MPa (gauge pressure), and the compound is obtained after 24 hours of reaction

[0044] Preparation step S2:

[0045]

[0046] Under the condition of stirring, add the above-mentioned 100g compound into the dry reactor of 1L Reaction solvent THF, tromethamine, compound The molar ratio with tromethamine is 1:3 respectively, the reaction temperature is 70°C, the reaction pressure is 0.1MPa (gauge pressure), and the reaction time is 5h. After the reaction was completed, the temperature was lowered to normal temperature, the insoluble matter was filtered off, the filtrate was evaporated under reduced pressure to remove the solvent, and concentrated to prepare th...

Embodiment 2

[0051] A preparation method of 1,3-bis(tri(hydroxymethyl)methylamino)propane, comprising the following preparation steps:

[0052] Preparation step S1:

[0053]

[0054] Under stirring conditions, add 100 g of 3-amino-1-propanol to a 1 L dry reactor, the reaction temperature is 180 ° C, the reaction pressure is 0.5 MPa (gauge pressure), and the reaction is 36 hours to obtain the compound

[0055] Preparation step S2:

[0056]

[0057] Under the condition of stirring, add the above-mentioned 100g compound into the dry reactor of 1L Reaction solvent acetonitrile, tromethamine, compound The molar ratio with tromethamine is 1:5 respectively, the reaction temperature is 85°C, the reaction pressure is 0.3MPa (gauge pressure), and the reaction time is 10h. After the reaction was completed, the temperature was lowered to normal temperature, the insoluble matter was filtered off, the filtrate was evaporated under reduced pressure to remove the solvent, and concentrated to ...

Embodiment 3

[0062] A preparation method of 1,3-bis(tri(hydroxymethyl)methylamino)propane, comprising the following preparation steps:

[0063] Preparation step S1:

[0064]

[0065] Under the condition of stirring, add 100g of 3-bromo-1-propanol into a 1L dry reactor, dissolve it in acetone solution, the reaction temperature is 60°C, the reaction pressure is 0.1MPa (gauge pressure), and react for 72h to obtain compound

[0066] Preparation step S2:

[0067]

[0068] Under the condition of stirring, add the above-mentioned 100g compound into the dry reactor of 1L Reaction solvent ethyl acetate, tromethamine, compound The molar ratio with tromethamine is 1:7 respectively, the reaction temperature is 80°C, the reaction pressure is 0.5MPa (gauge pressure), and the reaction time is 24h. After the reaction was completed, the temperature was lowered to normal temperature, the insoluble matter was filtered off, the filtrate was evaporated under reduced pressure to remove the solvent...

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Abstract

The invention discloses a preparation method of 1, 3-bis (tri (hydroxymethyl) methylamino) propane, which comprises the following steps: carrying out self reaction on a compound 1, or reacting the compound 1 with a condensation reagent to obtain a compound 2; and reacting the compound 2 with a compound 2A to obtain the 1, 3-bis (tri (hydroxymethyl) methylamino) propane, according to the method, the yield of the product is improved by optimizing the initial raw materials and optimizing the preparation and purification steps, the method is simple, the cost of the product is reduced, the method is suitable for industrial production, and the prepared 1, 3-bis (tris (hydroxymethyl) methylamino) propane is high in purity, has the advantages of low water content and dryness, meets the requirements of the biological buffering agent field on the purity, impurity content, cost and the like, and is suitable for industrial production. The method is suitable for application in the field of biological buffers.

Description

technical field [0001] The invention belongs to the technical field of biological buffers, in particular to a preparation method of 1,3-bis(tris(hydroxymethyl)methylamino)propane. Background technique [0002] 1,3-bis(tris(hydroxymethyl)methylamino)propane, the English name is 1,3-bis(tris(hydroxymethyl)methylamino)propane, also known as BIS-TRIS propane, is a white crystalline powder belonging to One of the TRIS series of biological buffers. The buffer range of BIS-TRIS propane is 6.3-9.5, at 25°C, its primary acid dissociation constant pKa 1 =6.8, the second-order acid dissociation constant pKa 2 =9.0. BIS-TRIS propane has been used in biochemical diagnostic kits, DNA / RNA extraction kits, and PCR diagnostic kits. It is one of the reagents with the highest application depth in the TRIS series products. [0003] In the preparation of BIS-TRIS propane, Chinese patent CN200810200543.2 discloses a preparation method, using trishydroxymethylaminomethane and 1,3-dibromopropan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/08C07C213/10C07C215/12C07D305/06C07D205/04C07D239/10C07D285/16C07D327/10C07D319/06
CPCC07C213/08C07C213/10C07D305/06C07D205/04C07D239/10C07D285/16C07D327/10C07D319/06C07C215/12
Inventor 袁永坤蒋玉贵顾临
Owner SUZHOU YACOO SCI CO LTD