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Preparation method of 1,1-cyclohexanediacetic acid

A kind of technology of cyclohexyl diacetic acid and cyclohexyl diacetic acid crude product, applied in 1 field, can solve the problems such as low product yield, environmental pollution, and three wastes are difficult to handle, and achieve high product yield, save equipment investment, and reduce production cost. Effect

Inactive Publication Date: 2009-07-08
曹桂东
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0016] In order to effectively solve problems such as low product yield, serious environmental pollution, and difficult disposal of the three wastes in the prior art, the inventor's purpose is to provide a kind of 1,1-cyclohexyl diacetic acid preparation method, in order to improve the product yield, At the same time, it is beneficial to environmental protection and reduces preparation time

Method used

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  • Preparation method of 1,1-cyclohexanediacetic acid
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  • Preparation method of 1,1-cyclohexanediacetic acid

Examples

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Effect test

Embodiment 1

[0070] (1) Preparation of 1,1-cyclohexyl dicyanoamide

[0071] Add 135ml of methanol into the reaction vessel, pass 10.5g of ammonia gas under the condition of cooling and stirring, cool down to -10°C, then add 51.5g of methyl cyanoacetate, the reaction temperature rises to -7°C, then cools down to -10°C, Add 25g of cyclohexanone dropwise (the temperature does not exceed -6°C during the dropwise addition), and drop it in about 40 minutes, then stir for half an hour, cool down to -10°C, stop stirring, and keep warm at -10°C for 24 hours, 0± Incubate at 5°C for 12 hours, at room temperature at 25°C for 12 hours (48 hours in total), filter the methanol solution with suction to obtain 1,1-cyclohexyl dicyanoamide, dry to obtain 1,1-cyclohexyldicyanoamide powder The pure 59.5g, yield 94.15%, enter the next step.

[0072] (2) Preparation of 1,1-cyclohexyl diacetic acid

[0073] (a) Add 70ml of water to the reaction vessel, slowly add 45ml of concentrated sulfuric acid, then add 59....

Embodiment 2

[0076] (1) Preparation of 1,1-cyclohexyl dicyanoamide

[0077] The mother liquor obtained by suction-filtering the methanol solution in step (1) of Implementation 1 is applied mechanically as follows: add 140ml of methanol mother liquor into the reaction vessel, feed 10g of ammonia gas under cooling and stirring conditions, cool down to -10°C, and then add cyanide Methyl acetate 51.5g, the temperature of the reaction was raised to -7°C, and then cooled to -10°C, 25g of cyclohexanone was added dropwise (the temperature did not exceed -6°C during the dropwise addition), and the drop was completed in about 40 minutes, stirred for half an hour, and cooled to -10°C, stop stirring, and then incubate at -10°C for 24 hours, at 0±5°C for 12 hours, and at room temperature 25°C for 12 hours (48 hours in total), and filter the methanol solution to obtain 1,1-cyclohexyldi Cyanamide was dried to obtain 60.6 g of pure 1,1-cyclohexyldicyanoamide powder, yield 95.88%, and proceeded to the next...

Embodiment 3

[0083] (1) Preparation of 1,1-cyclohexyl dicyanoamide

[0084] Add 140ml of absolute ethanol into the reaction vessel, pass 10.5g of ammonia gas under the condition of cooling and stirring, cool down to -10°C, then add 59.5g of ethyl cyanoacetate, the reaction temperature rises to -7°C, and then cools down to -10°C ℃, drop 25g of cyclohexanone (the temperature does not exceed -6 ℃ when dropping), drop it in about 40 minutes, then stir for half an hour, cool down to -10 ℃, stop stirring, and keep warm at -10 ℃ for 24 hours, Incubate at 0±5°C for 12 hours, at room temperature at 25°C for 12 hours (48 hours in total), filter the ethanol solution with suction to obtain 1,1-cyclohexyl dicyanoamide, and dry to obtain 1,1-cyclohexyl dicyanoamide The pure amide powder was 59.2 g, the yield was 93.67%, and the next step was carried out.

[0085] (2) Preparation of 1,1-cyclohexyl diacetic acid

[0086] (a) Add 70ml of water to the reaction vessel, slowly add 45ml of concentrated sulfu...

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Abstract

The invention discloses a method for preparing 1,1-cyclohexanediacetic acid. The preparation method has the following steps that: firstly, 1,1-cyclohexyl dicyanoamide is subjected to a hydrolysis reaction; secondly, paste obtained in the hydrolysis reaction is added into a sulphuric acid solution to carry out a decarboxylic reaction so as to prepare a 1,1-cyclohexanediacetic acid coarse product; and finally, the coarse product is refined to prepare the required product. Compared with the prior art, the method greatly reduces the preparation period, has higher product yield without the problem that 'the three wastes' is difficult to deal with, and contributes to environmental protection.

Description

technical field [0001] The invention relates to a preparation method of a gabapentin intermediate, in particular to a preparation method of 1,1-cyclohexyldiacetic acid. Background technique [0002] 1,1-Cyclohexanediacetic acid, also known as 1,1-cyclohexanediacetic acid or cyclohexanediacetic acid, is mainly used as an intermediate in the synthesis of antidepressant gabapentin. [0003] According to document record 1, the preparation method of 1-cyclohexyl diacetic acid is as follows: [0004] Step 1: Preparation of 1,1-cyclohexyl dicyanoamide [0005] Add methyl cyanoacetate (or ethyl cyanoacetate) and cyclohexanone in sequence in methanol (or absolute ethanol) solution, then cool down to about -10°C, and pass ammonia gas to react. From 10°C to 0°C and then to 25°C, the heat preservation reaction time is four days (ie 96 hours), and the methanol (or ethanol) solution is filtered with suction to obtain cyclohexyl dicyanoamide, which is dried and proceeds to the next step....

Claims

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Application Information

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IPC IPC(8): C07C55/28C07C51/06
Inventor 曹桂东吴伟荣
Owner 曹桂东
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