Synthetic method for drug intermediate acetonedicarboxylic acid

A technology of acetone dicarboxylic acid and a synthesis method, which is applied in the synthesis of acetone dicarboxylic acid pharmaceutical intermediates and the field of preparation of pharmaceutical intermediates, can solve problems such as health hazards for production operators, unfavorable safety production and the like, and achieves avoiding health hazards, Conducive to safe production and improved reaction yield

Inactive Publication Date: 2018-07-03
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, there is also a health hazard to the production operators, which is not conducive to safe production
Above-mentioned the

Method used

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  • Synthetic method for drug intermediate acetonedicarboxylic acid
  • Synthetic method for drug intermediate acetonedicarboxylic acid
  • Synthetic method for drug intermediate acetonedicarboxylic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] The synthetic method of acetone dicarboxylic acid medicine intermediate, comprises the steps:

[0016] A: Add 3mol 2-methoxypropane-1,3-dicarboxylic acid into the reaction vessel, 900ml mass fraction is 15% sodium nitrate solution, raise the temperature of the solution to 30°C, add 6mol in 2 times within 20min Lead tetraacetate, control stirring speed 150rpm, continue to react 80min;

[0017] B: Then add 6mol zinc oxalate powder, continue to react for 1h, lower the temperature to 15°C, add 10% potassium chloride solution for washing for 20 minutes, add 40% diphenyl ether solution for washing for 40 minutes, % recrystallized in diethylene glycol solution and dehydrated with anhydrous calcium sulfate dehydrating agent to obtain 427.926 g of finished acetone dicarboxylic acid with a yield of 97.7%.

Embodiment 2

[0019] The synthetic method of acetone dicarboxylic acid medicine intermediate, comprises the steps:

[0020] A: Add 3mol 2-methoxypropane-1,3-dicarboxylic acid into the reaction vessel, 900ml mass fraction is 18% sodium nitrate solution, raise the temperature of the solution to 33°C, add 7mol in 3 times within 30min Lead tetraacetate, control stirring speed 160rpm, continue to react 90min;

[0021] B: Then add 7mol zinc oxalate powder, continue the reaction for 1.5h, lower the temperature to 18°C, add a mass fraction of 13% potassium chloride solution for washing for 25 minutes, add a mass fraction of 44% diphenyl ether solution for washing for 50 minutes, Recrystallized in 63% diethylene glycol solution and dehydrated with anhydrous calcium sulfate dehydrating agent to obtain 428.802 g of acetone dicarboxylic acid with a yield of 97.9%.

Embodiment 3

[0023] The synthetic method of acetone dicarboxylic acid medicine intermediate, comprises the steps:

[0024] A: Add 3mol 2-methoxypropane-1,3-dicarboxylic acid into the reaction vessel, 900ml mass fraction is 22% sodium nitrate solution, raise the temperature of the solution to 36°C, add 8mol in 4 times within 40min Lead tetraacetate, control stirring speed 170rpm, continue to react 110min;

[0025] B: Then add 8 mol of zinc oxalate powder, continue to react for 2 hours, lower the temperature to 22°C, add a 16% potassium chloride solution for washing for 30 minutes, add a 47% diphenyl ether solution for washing for 60 minutes, and wash with a mass fraction of 65% % recrystallized in diethylene glycol solution and dehydrated with anhydrous calcium sulfate dehydrating agent to obtain 430.116 g of finished acetone dicarboxylic acid with a yield of 98.2%.

[0026] figure 1 It is the infrared analysis spectrogram of finished product acetone dicarboxylic acid.

[0027] Table 1 i...

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Abstract

The invention discloses a synthetic method for the drug intermediate acetonedicarboxylic acid. The synthetic method comprises the following steps: adding 2-methoxypropane-1,3-dicarboxylic acid and a sodium nitrate solution into a reaction vessel, increasing the temperature of the obtainded solution, adding lead tetraacetate in batches, controlling a stirring speed and continuing a reaction; and then adding zinc oxalate powder, continuing the reaction, carrying out cooling, carrying out washing with a potassium chloride solution, carrying out washing with a diphenyl ether solution, then carrying out recrystallization in a diethylene glycol solution, and carrying out dehydration with a dehydrating agent so as to obtain the finished acetonedicarboxylic acid.

Description

technical field [0001] The invention relates to a preparation method of a pharmaceutical intermediate, which belongs to the field of organic synthesis, in particular to a synthesis method of an acetone dicarboxylic acid pharmaceutical intermediate. Background technique [0002] As a pharmaceutical intermediate, acetone dicarboxylic acid is mainly used in anticholinergic drugs such as atropine and anisodamine. Most of the existing synthetic methods use citric acid as the raw material and deformation in the presence of concentrated sulfuric acid. First put oleum into the reaction tank, and then add citric acid under stirring. The proportion by weight is citric acid: fuming sulfuric acid, heat preservation reaction, then cooling down, centrifuging, rinsing with ice water, and drying to obtain the finished product. This synthesis method needs to use fuming sulfuric acid and citric acid as reaction raw materials, but the reaction raw material fuming sulfuric acid has a strong s...

Claims

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Application Information

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IPC IPC(8): C07C59/347C07C51/373
CPCC07C51/373C07C59/347
Inventor 严义达
Owner CHENGDU AO KA TE TECH CO LTD
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