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Synthesis method of vitamin A intermediate

A synthesis method and technology for intermediates, which are applied in the field of synthesis of vitamin A intermediates, can solve problems such as unsatisfactory results, and achieve the effects of reduced industrialization difficulty, easy large-scale production, and improved yield.

Pending Publication Date: 2022-04-12
GUANGZHOU WISDOM BIO TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] But the result is not ideal (Liu Jun. "Synthesis of 3-methyl-1-penten-4-yn-3-ol", Chemical Research and Application, Vol. 26 No. 9, September 2014), reported The gas phase yield is only 50%, and about 30% of the product is actually obtained, and a large amount of polymer is produced in the reaction process

Method used

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  • Synthesis method of vitamin A intermediate
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  • Synthesis method of vitamin A intermediate

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Experimental program
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Effect test

Embodiment 1

[0058] (1) butanone alcohol is dissolved in an organic solvent to make a butanone alcohol solution; the organic solvent is toluene, and the consumption adds 1ml by every gram of butanone alcohol;

[0059] (2) Control the temperature of the butanone alcohol solution to be 15° C. Under a nitrogen atmosphere and stirring conditions, add dropwise acetylene magnesium bromide-tetrahydrofuran solution to the butanone alcohol solution; after the addition is completed, continue to stir the reaction until the end of the reaction, and obtain Reaction solution; the concentration of acetylene magnesium bromide-tetrahydrofuran solution is 0.2M; the consumption of acetylene magnesium bromide-tetrahydrofuran solution is 1:2.2 according to the mol ratio of butanone alcohol and acetylene magnesium bromide in the whole material; The magnesium bromide-tetrahydrofuran solution was added dropwise in 2 hours; the reaction material was sampled and detected, and when the mass content of butanone alcoho...

Embodiment 2

[0069] Method is with embodiment 1, and difference is:

[0070] (1) The organic solvent is tetrahydrofuran, and the consumption is added 2ml per gram of butanone alcohol;

[0071] (2) control butanone alcohol solution temperature is 20 ℃; The concentration of acetylene magnesium bromide-tetrahydrofuran solution is 0.5M; The consumption of acetylene magnesium bromide-tetrahydrofuran solution is according to the mol ratio of butanone alcohol and acetylene magnesium bromide in the whole material The ratio is 1:2.3; the rate of addition is controlled by adding the acetylene magnesium bromide-tetrahydrofuran solution within 3 hours;

[0072] (3) The mass concentration of sulfuric acid solution is 10%; The consumption of sulfuric acid solution is 1: 6 by the volume ratio of distillate raffinate and sulfuric acid solution;

[0073] (4) The amount of dichloromethane is 1:6 according to the volume ratio of the mixed solution and dichloromethane;

[0074] (5) The solvent is n-hexane; ...

Embodiment 3

[0079] Method is with embodiment 1, and difference is:

[0080] (1) The organic solvent is n-hexane, and the consumption is added 2ml per gram of butanone alcohol;

[0081] (2) control butanone alcohol solution temperature is 25 ℃; The concentration of acetylene magnesium bromide-tetrahydrofuran solution is 0.8M; The consumption of acetylene magnesium bromide-tetrahydrofuran solution is according to the mol ratio of butanone alcohol and acetylene magnesium bromide in the whole material The ratio is 1:2.4; the rate of addition is controlled at the completion of the addition of the acetylene magnesium bromide-tetrahydrofuran solution within 3 hours;

[0082] (3) The mass concentration of sulfuric acid solution is 12%; The consumption of sulfuric acid solution is 1: 4 by the volume ratio of distillate raffinate and sulfuric acid solution;

[0083] (4) The amount of dichloromethane is 1:8 according to the volume ratio of the mixed solution and dichloromethane;

[0084] (5) The s...

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Abstract

The invention relates to a synthesis method of a vitamin A intermediate. The synthesis method comprises the following steps: (1) dissolving butanone alcohol in an organic solvent; (2) dropwise adding an acetylene magnesium bromide-tetrahydrofuran solution at the temperature of-25 DEG C to 50 DEG C in a nitrogen atmosphere under a stirring condition, and stirring to a reaction endpoint; (3) reduced pressure distillation; (4) mixing the distillation residual liquid with a sulfuric acid solution; (5) adding dichloromethane for extraction; (6) carrying out reduced pressure distillation on the extract; (7) dissolving the 3-methyl-3, 5-dihydroxy-1-pentyne in the solvent, and carrying out a reaction for 3-methyl-3, 5-dihydroxy-1-pentyne reaction; (8) adding dehydration acid, and carrying out distillation dehydration; (9) adding alkali liquor into the dehydrated material for neutralization, and performing oil-water separation to obtain a remaining oil phase; and (10) distilling the oil phase by using a distiller, wherein the part separated by distillation is the intermediate 3-methyl-2-pentene-4-alkyne-1-alcohol. Compared with an existing production process, the method has the advantages that the safety is improved, the industrialization difficulty is reduced, large-scale production is easy to realize, polymers are obviously reduced during ethynylation, and the yield is improved.

Description

technical field [0001] The invention belongs to the technical field of medicine and chemical industry, and in particular relates to a method for synthesizing a vitamin A intermediate. Background technique [0002] 3-Methyl-2-penten-4-yn-1-ol is a key intermediate in the synthesis of vitamin A and astaxanthin, and its synthesis research has always been highly concerned by technicians in this field. With the development of research Continuously deepening, but also made some progress. [0003] The reaction process of present industrialized production method is: [0004] [0005] In the above route, there are two great potential safety hazards in the process of preparing 3-methyl-1-pentene-4-yn-3-alcohol, that is, liquid ammonia is required as a reaction solvent, and the use of flammable metal lithium or Sodium is used for ethynylation; in order to overcome the above safety hazards, technicians use ethynyl Grignard reagents for ethynylation, as follows: [0006] [0007...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C33/048C07C29/60C07C29/74C07C29/80
Inventor 邸维龙黄海青梁庭枝张贵东江华峰吴世林
Owner GUANGZHOU WISDOM BIO TECH
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