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Synthetic method of 2,3-dihydrobutanedioic acid drug intermediate

A technology of dihydroxysuccinic acid and synthesis method, which is applied in the field of organic synthesis, can solve problems such as unfavorable safety production, endangering the health of production operators, etc., and achieve the effects of reducing intermediate links, shortening reaction time, and improving reaction yield

Inactive Publication Date: 2018-07-17
CHENGDU AO KA TE TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the use of hydrocyanic acid as a reaction raw material will seriously endanger the health of production operators and is not conducive to safe production.

Method used

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  • Synthetic method of 2,3-dihydrobutanedioic acid drug intermediate
  • Synthetic method of 2,3-dihydrobutanedioic acid drug intermediate
  • Synthetic method of 2,3-dihydrobutanedioic acid drug intermediate

Examples

Experimental program
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Effect test

Embodiment 1

[0017] The synthetic method of 2,3-dihydroxysuccinic acid pharmaceutical intermediate comprises the steps:

[0018] A: Add 3mol 1,4-dibromo-2,3-dimethoxy-butanedialdehyde in the reaction vessel, 900ml mass fraction is 15% heptane solution, control the stirring speed to 170rpm, raise the solution temperature to 40°C , add 6 mol aqueous solution, 6 mol dimethyl sulfoxide, add 6 mol mass fraction of 20% dioctyl sebacate solution in 2 times within 20 minutes, and continue the reaction for 50 minutes;

[0019] B: Raise the temperature to 55°C, add 1.3L of 10% potassium bromide solution and 3mol of zinc acetate powder, continue the reaction for 2 hours, lower the temperature to 10°C, let stand for 30min, add 700ml of 20% sodium nitrate Solution, the solution is separated, the oil layer is separated, washed with a 40% 3-hexanol solution for 30 minutes, recrystallized in a 60% cyclopentanoic acid solution, and dehydrated with anhydrous magnesium sulfate dehydrating agent to obtain the...

Embodiment 2

[0021] The synthetic method of 2,3-dihydroxysuccinic acid pharmaceutical intermediate comprises the steps:

[0022] A: Add 3mol 1,4-dibromo-2,3-dimethoxy-butanedialdehyde in the reaction vessel, 900ml mass fraction is 18% heptane solution, control the stirring speed at 180rpm, raise the solution temperature to 43°C , add 7mol aqueous solution, 7mol dimethyl sulfoxide, add 7mol mass fraction of 23% dioctyl sebacate solution in 3 times within 30min, continue to react for 70min;

[0023] B: Raise the temperature to 58°C, add 1.3L of 13% potassium bromide solution and 4mol zinc acetate powder, continue the reaction for 2.5h, lower the temperature to 13°C, let stand for 40min, add 700ml of 23% nitric acid Sodium solution, the solution is separated, the oil layer is separated, washed with 43% 3-hexanol solution for 40 minutes, recrystallized in 64% cyclopentanoic acid solution, dehydrated with anhydrous magnesium sulfate dehydrating agent, and the finished product 2 is obtained. , ...

Embodiment 3

[0025] The synthetic method of 2,3-dihydroxysuccinic acid pharmaceutical intermediate comprises the steps:

[0026] A: Add 3mol 1,4-dibromo-2,3-dimethoxy-butanedialdehyde in the reaction vessel, 900ml mass fraction is 21% heptane solution, control the stirring speed at 190rpm, raise the solution temperature to 46°C , add 8 mol aqueous solution, 8 mol dimethyl sulfoxide, add 8 mol mass fraction of 26% dioctyl sebacate solution in 4 times within 40 minutes, and continue the reaction for 80 minutes;

[0027] B: Raise the temperature to 62°C, add 1.3L of 15% potassium bromide solution and 5mol of zinc acetate powder, continue the reaction for 3 hours, lower the temperature to 16°C, let stand for 50min, add 700ml of 26% sodium nitrate solution, the solution was separated, the oil layer was separated, washed with a 45% 3-hexanol solution for 50 minutes, recrystallized in a 67% cyclopentanoic acid solution, and dehydrated with anhydrous magnesium sulfate dehydrating agent to obtain t...

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Abstract

The invention discloses a synthetic method of a 2,3-dihydrobutanedioic acid drug intermediate. The synthetic method comprises the following steps: adding 1,4-dibromo-2,3-dimethoxy-butanedial and a heptane solution into a reaction container, controlling the stirring speed to be 170 to 190 rpm, increasing the temperature to be 40 to 46 DEG C, adding a water solution and dimethyl sulfoxide, adding adioctyl sebacate solution within 20 to 40 min in batches, and continuously reacting for 50 to 80 min; increasing the temperature to be 55 to 62 DEG C, adding a potassium bromide solution and zinc acetate powder, continuously reacting for 2 to 3 h, reducing the temperature to be 10 to 16 DEG C, leaving to stand for 30 to 50 min, adding a sodium nitrate solution, layering the solution to separate anoil layer, washing with a 3-hexyl alcohol solution for 30 to 50 min, carrying out recrystallization in a cyclopentanecarboxylic acid solution, and carrying out dehydration by a dehydrating agent to obtain the finished product 2,3-dihydrobutanedioic acid.

Description

technical field [0001] The invention relates to a preparation method of a pharmaceutical intermediate, belonging to the field of organic synthesis, in particular to a synthesis method of a 2,3-dihydroxysuccinic acid pharmaceutical intermediate. Background technique [0002] 2,3-Dihydroxysuccinic acid is mainly used in medicine, food, leather, textile and other industries, as antioxidant synergist, retarder, tanning agent, chelating agent, pharmaceutical; 2,3-Dihydroxybutane Diacids are very important chiral ligands and chiralons that can be used to prepare many well-known chiral catalysts and as chiral sources to synthesize complex natural product molecules. Most of the existing synthetic methods are obtained by reacting glyoxal with hydrocyanic acid and then acid hydrolysis. The reaction raw material glyoxal used in this synthetic method is harmful to human body if inhaled, ingested or absorbed through the skin; it has a stimulating effect on the skin , can cause dermatiti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/04C07C51/367C07C59/245C07C59/255
CPCC07C51/04C07C51/367C07C59/245C07C59/255
Inventor 严义达
Owner CHENGDU AO KA TE TECH CO LTD
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