Preparation of 1,3-bis[(trihydroxymethyl) methyl amino] propane

A technology of tris(hydroxymethyl)aminomethane and methylamino, which is applied in 1 field to achieve the effects of optimizing preparation process conditions and processes, and high yield

Inactive Publication Date: 2009-03-04
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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But, about 1, the preparation method of 3-bis [(tr...

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  • Preparation of 1,3-bis[(trihydroxymethyl) methyl amino] propane

Examples

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Embodiment 1

[0017] Add trishydroxymethylaminomethane and 1,3-dibromopropane at a molar ratio of 1:1 to 1500ml ethanol solution, react under reflux for 6 hours, and stand at room temperature for 12 hours to form trishydroxymethylaminomethane bromide Needle crystals of hydrogen, vacuum filtration, acidification of the filtrate with HBr to pH = 1.5, cryogenic crystallization to obtain 1,3-bis[(trimethylol)methylamino]propane 2HBr crystals, vacuum filtration, The filter cake was dissolved in absolute ethanol, adjusted to pH = 11.0 with NaOH, cryogenically crystallized, and dried to obtain crude 1,3-bis[(trimethylol)methylamino]propane. Dissolve the crude product in hot absolute ethanol, cool naturally, vacuum filter, remove insoluble matter, stand at room temperature for 6 hours to crystallize, repeat the above recrystallization three times, vacuum filter, and vacuum dry at 50-60°C to obtain Pure 1,3-bis[(trimethylol)methylamino]propane product. The reaction yield is 30%, the product purity ...

Embodiment 2

[0019] Add trishydroxymethylaminomethane and 1,3-dibromopropane at a molar ratio of 2:1 to 1500ml ethanol solution, react under reflux for 4 hours, cryogenically crystallize for 2 hours, and form trishydroxymethylaminomethane·hydrogen bromide Needle-shaped crystals of 1,3-bis[(trimethylol)methylamino]propane 2HBr crystals were obtained by vacuum filtration, and the filtrate was acidified to pH=3.0 by adding HBr to the filtrate. The cake was dissolved in absolute ethanol, adjusted to pH = 9.0 with NaOH, cryogenically crystallized, and dried to obtain crude 1,3-bis[(trimethylol)methylamino]propane. Dissolve the crude product in hot absolute ethanol, cool naturally, vacuum filter, remove insoluble matter, stand at room temperature for 6 hours to crystallize, repeat the above recrystallization three times, vacuum filter, and vacuum dry at 50-60°C to obtain Pure 1,3-bis[(trimethylol)methylamino]propane product. The reaction yield was 45%, the product purity was 92.0%, and the melt...

Embodiment 3

[0021] Add trishydroxymethylaminomethane and 1,3-dibromopropane in a molar ratio of 4:1 to 1500ml ethanol solution, react for 9 hours under reflux, and stand at room temperature for 12 hours to form trishydroxymethylaminomethane bromide Needle crystals of hydrogen, vacuum filtration, acidification of the filtrate with HBr to pH=2.0, cryogenic crystallization to obtain 1,3-bis[(trimethylol)methylamino]propane 2HBr crystals, vacuum filtration, The filter cake was dissolved in absolute ethanol, adjusted to pH = 10.0 with NaOH, cryogenically crystallized, and dried to obtain crude 1,3-bis[(trimethylol)methylamino]propane. Dissolve the crude product in hot absolute ethanol, cool naturally, vacuum filter, remove insoluble matter, stand at room temperature for crystallization, repeat the above recrystallization three times, vacuum filter, and vacuum dry at 50-60°C to obtain pure 1,3-bis[(trimethylol)methylamino]propane product. The reaction yield was 60%, the product purity was 99.5...

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Abstract

The invention discloses a method for preparing 1,3-bis[(trihydroxy)methylamino]propane. The method comprises the following steps: adopting trihydroxymethyl aminomethane and 1,3-dibromopropane as the main reaction materials; reacting in an ethanol solution under reflux for a certain time; respectively subjecting to the acidification and the alkalization treatment to obtain a coarse target product; and re-crystallizing to obtain a pure product. The method has the advantages that the preparation condition and process are optimized; the yield is 30% to 80% in terms of the ratio of an actual yield to a theoretical yield, and the product purity is 90% to 99.5% and the melting point is 164 to 165 DEG C..

Description

【Technical field】 [0001] The invention relates to the field of fine chemicals, in particular to a preparation method of 1,3-bis[(trimethylol)methylamino]propane. 【Background technique】 [0002] 1,3-bis[(trimethylol)methylamino]propane (1,3-Bis-[-tris-(hydrolymethyl)-methylamino]-propane or Bis-Tris Propane, BTP for short) is a zwitterion Buffer, due to the existence of two very close pKa values ​​of 6.8 and 9.0, thus has a strong buffer capacity, and its buffer range is pH=6.3 to 9.5, and is widely used in the fields of biochemistry and molecular biology, such as in polymerase chain reaction BTP can be used as a stable buffer [Eckert, K.A., and Kunkel, T.A., DNA polymerase fidelity and the polymerase chainreaction[J]. PCR Methods Appl., 1991; 1(1):17-24], BTP / HCl buffer Farnesyl diphosphate accumulation in yeast ERG9 mutants [Song, L., Detection of farnesyldiphosphate accumulation in yeast ERG9 mutants [J]. Anal. Biochem., 2003; 317 (2): 180- 185]. BTP buffer can be used ...

Claims

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Application Information

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IPC IPC(8): C07C215/10C07C213/08
Inventor 许振良王靖宇张勤岳吴萍张颖魏永明吴永阳
Owner EAST CHINA UNIV OF SCI & TECH
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