Preparation method of 3,3-pentamethylene glutarimide

A technology of cyclopentane glutarimide and cyclohexyl diacetic acid monoamide, applied in the direction of organic chemistry, can solve the problems of incompleteness, low product content, low yield, etc., and achieve low loss of raw materials and source of raw materials Broad, low-polluting effect

Inactive Publication Date: 2013-12-18
JIANGSU RUIDA TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The content of the product obtained in this way will not be very high, the main reason is that the content of the product is not high and the yield is low due to the incomplete anhydride process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0019] The preparation method of 3,3-cyclopentane glutarimide disclosed by the present invention comprises the following steps: a), configuring stirring equipment and azeotropic fractionation equipment for the reactor, and putting raw material 1,1-cycloglutarimide into the reactor Hexyl diacetic acid monoamide, solvent toluene and catalyst glacial acetic acid, wherein the molar ratio of substances is n (1,1-cyclohexyl diacetic acid monoamide): n (toluene): n (glacial acetic acid)=1:1.5-3: 0.1-0.2, the temperature is raised to reflux, and the reaction shown in formula (I) takes place in the reactor; b), reflux at 100-130°C to separate water, react for 18-26 hours, stop heating, and stir slowly to cool down to room temperature, then filter cake by suction filtration; c), put the filter cake obtained by suction filtration into dilute ammonia water After soaking, beating and stirring for 3-4 hours, suction filtration, then rinse the filter cake obtained by suction filtration with...

Embodiment 1

[0031] Configure stirring equipment and azeotropic fractionation equipment for the reactor, then drop into the reactor raw material 1,1-cyclohexyl diacetic acid monoamide, solvent toluene and catalyst glacial acetic acid, wherein the molar ratio of the substances is n(1,1-cyclo Hexyl diacetic acid monoamide): n (toluene): n (glacial acetic acid) = 1: 1.5: 0.1, heat up to reflux; reflux at 100 ° C to separate water, react for 18 hours, stop heating, and slowly cool down to room temperature after stirring , the cooling rate was 1°C / min, and the filter cake was obtained by suction filtration; the filter cake obtained by suction filtration was put into dilute ammonia water with a concentration of 13%, soaked, beaten and stirred for 3 hours, then suction filtered, and then the filter cake obtained by suction filtration was used Rinse with clean water 3 times, and the amount of clean water used for each rinse is n (water): n(1,1-cyclohexyl diacetic acid monoamide)=0.4:1 to obtain the...

Embodiment 2

[0033] Recycling the toluene mother liquor obtained by suction filtration in Example 1 is replenished until the feed ratio is n(1,1-cyclohexyl diacetic acid monoamide):n(toluene)=1:1.5, and other synthesis conditions and processes are the same as in Example 1 As described above, the yield is 93.8%, and the content (HPLC) is 99.8%. The melting range of the product is mp: 168-171°C.

[0034] The toluene mother liquor obtained by suction filtration involved in the present invention can be recovered and recycled multiple times, and is not limited to the two utilizations shown in the first and second examples.

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PUM

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Abstract

The invention discloses a preparation method of 3,3-pentamethylene glutarimide. According to a formula (I), 1,1-cyclohexanediacetic acid mono amide as a raw material, toluene as a solvent and glacial acetic acid as a catalyst undergo a reaction to produce the 3,3-pentamethylene glutarimide as a gabapentin intermediate. The preparation method improves reaction raw material amidation efficiency, a product yield and an output. The preparation method utilizes toluene as the reaction solvent and glacial acetic acid as the catalyst so that reaction efficiency is improved and a product yield is improved. Through recycle of a filtration mother liquor of a main reaction, a production cost is reduced and production benefits are improved.

Description

[0001] technical field [0002] The invention relates to a synthesis method of a fine chemical gabapentin pharmaceutical intermediate, in particular to a preparation method of 3,3-cyclopentane glutarimide. Background technique [0003] There are many synthesis methods related to gabapentin in the prior art, for example, in patent documents such as U.S. Pat. Nos. 5,132,451, 5,095,148, 5,068,413, a large number of related synthesis technologies of this product have been disclosed. However, due to the use of cyanide-containing intermediates, special strict conditions are required to hydrogenate them. At the same time, due to the great toxicity of cyanide-containing organic materials, the requirements for production environment and production equipment are relatively high. In addition, react with 1,1-cyclohexyl diacetic acid, acetic anhydride, ammonium acetate, etc., and then obtain the product through refining. The content of the product obtained in this way will not be ve...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D221/20
Inventor 陆孙彬周乔周士涛
Owner JIANGSU RUIDA TECH CO LTD
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