Preparation method of 3,3-dimethyl-1,2-cyclopropane dicarboxylic acid

A technology of cyclopropanedicarboxylic acid and dimethyl, which is applied in the field of chemical synthesis, can solve the problems of high production cost, achieve the effects of reducing production cost, broadening the application range, and shortening the reaction route

Inactive Publication Date: 2014-12-24
WUZHOU CAYIN GUM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of this invention is to provide a kind of preparation method of 3,3-dimethyl-1,2-cyclopropane dicarboxylic acid, this method is raw material with 3-carene, the purpose is to solve 3,3-dimethyl-1,2-cyclopropanedicarboxylic acid The problem of high production cost of 1,2-cyclopropanedicarboxylic acid

Method used

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  • Preparation method of 3,3-dimethyl-1,2-cyclopropane dicarboxylic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 100 grams of 3-carene, 5 grams of cetyl sodium sulfate and 350 grams of water to the reaction kettle in turn, gradually add 600 grams of potassium permanganate to the reaction kettle, and finish adding in 3 hours, stir evenly, and control the reaction temperature 35°C, react for 5 hours; filter, collect the filtrate and filter residue respectively, the filtrate is set aside, add water to the filter residue and wash 8 times, collect the washing liquid, combine the filtrate and washing liquid to obtain a mixed solution, adjust the pH value of the mixed solution to 10, and add to the mixed solution Add 1 / 4 volume of benzene to the solution to extract 3 times, collect the aqueous layer solution, add 0.1mol / L hydrochloric acid solution to the aqueous layer solution to adjust the pH of the solution to 2, heat and concentrate at 90°C, filter, wash with water, and dry , That is, 3,3-dimethyl-1,2-cyclopropane dicarboxylic acid.

Embodiment 2

[0023] Add 1 kilogram of 3-carene, 50 grams of cetyl sodium sulfate and 10 kilograms of water to the reaction kettle in turn, gradually add 2.5 kilograms of potassium permanganate to the reaction kettle, finish adding in 3 hours, stir evenly, and control the reaction temperature at 20°C, react for 10 hours; filter, collect the filtrate and filter residue respectively, the filtrate is set aside, add water to the filter residue and wash 8 times, collect the washing liquid, combine the filtrate and washing liquid to obtain a mixed solution, adjust the pH value of the mixed solution to 10, and add to the mixed solution Add 1 / 4 volume of benzene to the solution to extract 5 times, collect the aqueous layer solution, add 0.1mol / L hydrochloric acid solution to the aqueous layer solution to adjust the pH to 2, heat and concentrate at 90°C, filter, wash with water, and dry. That is, 3,3-dimethyl-1,2-cyclopropane dicarboxylic acid.

Embodiment 3

[0025] Add 10 kilograms of 3-carene, 100 grams of cetyl sodium sulfate and 70 kilograms of water to the reaction kettle in turn, gradually add 90 kilograms of potassium permanganate to the reaction kettle, and finish adding in 3 hours, stir evenly, and control the reaction temperature 5°C, reacted for 15 hours; filtered, collected the filtrate and filter residue respectively, the filtrate was set aside, the filter residue was washed with water 8 times, the washing liquid was collected, the filtrate and the washing liquid were combined to obtain a mixed solution, and the pH value of the mixed solution was adjusted to 10. Add 1 / 4 volume of benzene to the solution to extract 4 times, collect the aqueous layer solution, add 0.1mol / L hydrochloric acid solution to the aqueous layer solution to adjust the pH of the solution to 2, heat and concentrate at 90°C, filter, wash with water, and dry , That is, 3,3-dimethyl-1,2-cyclopropane dicarboxylic acid.

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Abstract

The invention discloses a preparation method of 3,3-dimethyl-1,2-cyclopropane dicarboxylic acid, which comprises the following steps: sequentially adding 3-carene, cetyl sodium sulfate and water into a reactor, gradually adding potassium permanganate into the reactor, stirring uniformly, regulating the temperature of the reactor, carrying out oxidation reaction, filtering, collecting the filtrate and filtration residue for later use, washing the filtration residue with water, collecting the washing solution, merging the filtrate and washing solution to obtain a mixed solution, regulating the pH value of the mixed solution, adding benzene for extraction, collecting the water layer solution, regulating the pH value of the water layer solution, heating for concentration, filtering, washing with water, and drying to obtain the 3,3-dimethyl-1,2-cyclopropane dicarboxylic acid. By preparing the 3,3-dimethyl-1,2-cyclopropane dicarboxylic acid from the 3-carene, the method shortens the reaction route and lowers the production cost.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a preparation method of 3,3-dimethyl-1,2-cyclopropanedicarboxylic acid. Background technique [0002] 3,3-Dimethyl-1,2-cyclopropanedicarboxylic acid is an ideal raw material for synthetic drugs, and its molecular formula is C 7 h 10 o 4 , the structural formula is as follows: [0003] [0004] At present, the synthesis of 3,3-dimethyl-1,2-cyclopropanedicarboxylic acid is prepared from chrysanthemic acid ester through oxidation, saponification and acidification. Raw materials are expensive, which ultimately leads to higher production costs of 3,3-dimethyl-1,2-cyclopropanedicarboxylic acid. [0005] Contents of the invention [0006] The purpose of this invention is to provide a kind of preparation method of 3,3-dimethyl-1,2-cyclopropane dicarboxylic acid, this method is raw material with 3-carene, the purpose is to solve 3,3-dimethyl-1,2-cyclopropanedicarb...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/31C07C61/04
CPCC07C51/31C07C51/02C07C51/48C07C2601/02C07C61/04
Inventor 杨韶平陈伟强陈键泉董俊刘娟娟谭育慧
Owner WUZHOU CAYIN GUM
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