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Preparation process for L-lyxose

A preparation process and lyxose technology, applied in the field of L-lyxose preparation, can solve the problems of complex source of raw materials, difficulty in large-scale production, difficulty in realizing large-scale production, etc. Easy to use effect

Active Publication Date: 2019-02-12
浙江晟格生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In these methods, it is obtained from relatively simple raw materials through multi-step protection and deprotection, oxidation removal of terminal C-C bonds, or the sources of raw materials are complex, and it is difficult to achieve large-scale production
[0007] In summary, in order to solve the problems existing in the prior art that the relatively simple raw materials are obtained through multi-step protection and deprotection, and the terminal C-C bonds are removed by oxidation, or the source of the raw materials is complicated, and it is difficult to realize large-scale production, it is urgent to invent a A new artificially synthesized L-lyxose preparation process with cheap and easy-to-obtain raw materials, simple and safe operation, and high-purity products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A preparation process of L-lyxose, comprising the following steps:

[0026] Step 1, the synthesis of intermediate material 1-methyl-D-ribose: put 325ml of anhydrous methanol into the reaction kettle, add 60g of D-ribose under the condition of stirring, and dropwise add 3g of sulfuric acid, control the temperature at 60-65 degrees, After mixing evenly, heat and reflux for 12 hours; TLC tracking, after the reaction is completed, adjust the pH to 6-7 with sodium carbonate, then filter, and concentrate the filtrate to dryness to 80g for later use;

[0027] Step 2, the synthesis of intermediate material 2,3-propylidene-methyl-D-ribose: add acetone 350ml, 2,2-dimethoxypropane 50ml and concentrated sulfuric acid 1ml to the concentrated filtrate 80g in step 1, and the solution is in Stir vigorously at room temperature for 50 minutes, then add 10 g of calcium carbonate, and stir the resulting suspension at room temperature for 50 minutes, then filter the suspension, wash the sol...

Embodiment 2

[0032] A preparation process of L-lyxose, comprising the following steps:

[0033] Step 1, the synthesis of 1-methyl-D-ribose: Put 400ml of anhydrous methanol into the reaction kettle, add 80g of D-ribose under stirring conditions, and dropwise add 4g of sulfuric acid, control the temperature at 60-65 degrees, and mix well Afterwards, heat and reflux for 12 hours; TLC tracking, after the reaction is completed, use sodium carbonate to adjust PH=6-7, then filter, and the filtrate is concentrated to dryness to 100 g for later use;

[0034] Step 2, the synthesis of 2,3-propylidene-methyl-D-ribose: add 250ml of acetone, 30ml of 2,2-dimethoxypropane and 1ml of concentrated sulfuric acid to 100g of the concentrated filtrate in step 1, and the solution is at room temperature Stir vigorously for 50 minutes, then add 5 g of calcium carbonate, and stir the resulting suspension at room temperature for 50 minutes, then filter the suspension, wash the solid with 50 ml of acetone, and concen...

Embodiment 3

[0039] A preparation process of L-lyxose, comprising the following steps:

[0040] Step 1, the synthesis of 1-methyl-D-ribose: Put 300ml of anhydrous methanol into the reaction kettle, add 50g of D-ribose under the condition of stirring, and dropwise add 2g of sulfuric acid, control the temperature at 63 degrees, mix well, Heat to reflux for 12 hours; TLC tracking, after the reaction is completed, adjust the pH to 6-7 with sodium carbonate, then filter, and concentrate the filtrate to 60 g for later use;

[0041] Step 2, the synthesis of 2,3-propylidene-methyl-D-ribose: add 250ml of acetone, 30ml of 2,2-dimethoxypropane and 1ml of concentrated sulfuric acid to 600g of the concentrated filtrate in step 1, and the solution is at room temperature Stir vigorously for 50 minutes, then add 5 g of calcium carbonate, and stir the resulting suspension at room temperature for 50 minutes, then filter the suspension, wash the solid with 50 ml of acetone, and concentrate the washed filtrat...

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Abstract

The invention belongs to the technical field of L-lyxose preparation, and relates in particular to a preparation process for L-lyxose. The preparation process comprises the following steps: synthesisofzing 1-methyl-D-ribose, synthesis of 2,3-propylidene-methyl-D-ribose, synthesis of 2,3-propylidene-methylsulfonyl-mthyl-D-ribose, and synthesis of 2,3-propylidene-methyl-L-lyxose and L-lyxose. Thepreparation process for the L-lyxose takes D-ribose as the raw material, and is used for synthesizing L-lyxose by methyl conversion, propylidene conversion, protective group (methylsulfonyl) conversion, and conversion de-protection, so that L-lyxose is prepared through D to L conversion and methyl and propylidene desorption. The whole preparation process is high in catalysisconversion efficiency,is relatively simple in process, adopts cheap and easily available raw materials, is simple and convenient to operate, and is safe; and the obtained product is high in purity.

Description

technical field [0001] The invention relates to a preparation process of L-lyxose, which is applicable to some new artificially synthesized L-lyxose preparation processes. It belongs to the technical field of L-lyxose preparation. Background technique [0002] According to the information of the International Rare Sugar Society, the currently known rare monosaccharides include: L-ribulose, L-xylose, L-lyxose, L-psicose, etc. The distribution of rare monosaccharides in nature is very rare, but because these monosaccharides have some special physical and chemical properties, they have gained widespread attention and popularity in the scientific and technological circles. As one of the rare five-carbon sugars, L-lyxose is mainly obtained by multi-step chemical synthesis in addition to biological enzyme catalysis. However, the current method for chemically synthesizing L-lyxose is cumbersome, or the sources of raw materials are complicated. Therefore, it is of great significan...

Claims

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Application Information

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IPC IPC(8): C07H3/02C07H1/00
CPCC07H1/00C07H3/02C07B2200/07Y02P20/55
Inventor 陈红辉
Owner 浙江晟格生物科技有限公司
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