Organic synthesis raw material valeric acid synthesis method

A technology of organic synthesis and synthesis method, which is applied in the field of synthesis of valeric acid, a raw material for organic synthesis, can solve problems such as low yield and complicated process, and achieve the effects of shortening reaction time, reducing intermediate links, and improving reaction yield

Inactive Publication Date: 2018-07-03
CHENGDU DONG DIAN AI ER TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] Valeric acid is mainly used in the production of valeric acid esters, as raw materials for spices and as raw materials for estrogen estradiol valeric acid esters and disinfectants, but most of the existing synthetic methods use formic acid and 1-butene to react to generate n-valeric acid , the process is more complicated, and the final yield is not very high. Therefore, it is necessary to propose a new synthetic method, which has important economic significance for further improving the quality and yield of the product and reducing the content of by-products

Method used

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  • Organic synthesis raw material valeric acid synthesis method

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Effect test

example 1

[0010] Add 3mol of methyl propyl ketone and 4mol of tributyl citrate solution with a mass fraction of 70% in the reaction vessel, control the stirring speed at 190rpm, lower the solution temperature to 6°C, keep it for 60min, and then increase the solution temperature to 10°C , add 3 mol of chromium acetate in 3 times, each interval of 30min, continue to react for 2h, then let it stand for 60min, add 300ml of potassium nitrate solution with a mass fraction of 20%, the solution is layered, and the water layer is 70% with a mass fraction of The 4-heptanone solution was extracted 3 times, the mass fraction was 80% 3-methyl-2-pentanone solution extracted 4 times, the oil layer and the extract were combined, and the mass fraction was 90% isobutyl butyrate solution. Crystallized and dehydrated with anhydrous magnesium sulfate dehydrating agent to obtain 240.24 g of finished valeric acid with a yield of 91%.

example 2

[0012] Add 3mol of methyl propyl ketone and 5mol of tributyl citrate solution with a mass fraction of 75% in the reaction vessel, control the stirring speed to 210rpm, lower the solution temperature to 7°C, keep it for 70min, and then increase the solution temperature to 12°C , add 3.5mol of chromium acetate in 5 times, each time interval is 35min, continue to react for 2.5h, then let it stand for 70min, add 300ml of potassium nitrate solution with a mass fraction of 23%, the solution is layered, and the water layer uses a mass fraction of 72% % 4-heptanone solution was extracted 4 times, the mass fraction was 85% 3-methyl-2-pentanone solution was extracted 5 times, the oil layer and the extract were combined, and the mass fraction was 93% isobutyl butyrate solution Medium recrystallization, dehydration with anhydrous potassium carbonate dehydrating agent, 245.52 g of finished valeric acid was obtained, yield 93%.

example 3

[0014] Add 3mol of methyl propyl ketone and 6mol of tributyl citrate solution with a mass fraction of 78% in the reaction vessel, control the stirring speed at 220rpm, lower the solution temperature to 9°C, keep it for 80min, then increase the solution temperature to 15°C , add 4mol of chromium acetate in 6 times, each interval of 40min, continue to react for 3h, then let it stand for 80min, add 300ml of potassium nitrate solution with a mass fraction of 26%, the solution is layered, and the water layer is 75% with a mass fraction of The 4-heptanone solution was extracted 5 times, the mass fraction was 88% 3-methyl-2-pentanone solution was extracted 6 times, the oil layer and the extract were combined, and the mass fraction was 96% in isobutyl butyrate solution. Crystallized and dehydrated with anhydrous magnesium sulfate dehydrating agent to obtain 253.44 g of finished valeric acid with a yield of 96%.

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Abstract

The invention relates to an organic synthesis raw material valeric acid synthesis method, which mainly comprises: adding 3 mol methyl propyl ketone and 4-6 mol tributyl citrate solution to a reactioncontainer, controlling the stirring speed at 190-220 rpm, reducing the solution temperature to 6-9 DEG C, maintaining for 60-80 min, increasing the temperature of the solution to 10-15 DEG C, adding 3-4 mol chromium acetate in 3-6 times every 30-40 min, continuously carrying out the reaction for 2-3 h, standing for 60-80 min, adding 300 ml of a potassium nitrate solution, layering the solution, extracting 3-5 times with a 4-heptanone solution, extracting 4-6 times with a 3-methyl-2-pentanone solution, combining the oil layer and the extraction liquid, re-crystallizing in an isobutyl butyrate solution, and dehydrating with a dehydrating agent to obtain the finished product valeric acid.

Description

technical field [0001] The invention relates to a method for synthesizing valeric acid as an organic synthesis raw material. Background technique [0002] Valeric acid is mainly used in the production of valeric acid esters, as raw materials for spices and as raw materials for estrogen estradiol valeric acid esters and disinfectants, but most of the existing synthetic methods use formic acid and 1-butene to react to generate n-valeric acid , the process is relatively complicated, and the final yield is not very high. Therefore, it is necessary to propose a new synthetic method, which has important economic significance for further improving the quality and yield of the product and reducing the content of by-products. Contents of the invention [0003] The object of the present invention is to provide a kind of synthetic method of organic synthesis raw material valeric acid, comprises the steps: [0004] (i) Add 3mol of methyl propyl ketone and 4-6mol of tributyl citrate s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/00C07C53/124
CPCC07C51/00C07C53/124
Inventor 严义达
Owner CHENGDU DONG DIAN AI ER TECH
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