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Synthetic process for sodium gualenate monohydrate

A technology of sodium azulene sulfonate and monohydrate, which is applied in the field of chemical synthesis, can solve the problems that the sodium azulene sulfonate has not been retrieved, and the research on the preparation of sodium azulene sulfonate crystal hydrate is still blank, etc., and achieves the effect of reducing pollution.

Active Publication Date: 2017-05-31
NANJING GRITPHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] No method for preparing sodium azulene sulfonate monohydrate has been retrieved yet, and the research on the preparation of sodium azulene sulfonate crystalline hydrate is still blank

Method used

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  • Synthetic process for sodium gualenate monohydrate
  • Synthetic process for sodium gualenate monohydrate
  • Synthetic process for sodium gualenate monohydrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] The synthetic method of sodium azulene sulfonate monohydrate is shown in the following equation:

[0046]

[0047] Add 20g of sodium azulene sulfonate to a 500ml three-necked flask, add 200ml of water and stir for 30 minutes, raise the internal temperature to 85°C and reflux for 2 hours. After reflux for 2 hours, place the system in an ice bath and continue stirring for 2 hours. crystal.

[0048] The precipitated crystals were suction-filtered with a Buchner funnel, washed twice with 150 ml of water, and suction-filtered, and the filter cake was vacuum-dried at 35°C to constant weight to obtain 14 g of sodium azulenesulfonate hemihydrate. Dry to constant weight, and detect moisture content with Karl Fischer moisture analyzer to be 3.06%, the result is as follows: figure 1 As shown, the TG test results are as follows figure 2 shown.

[0049] Add 14g sodium azulene sulfonate hemihydrate into a 500mL three-necked flask, add a mixed solution of 70mL water and 70mL pe...

Embodiment 2

[0056] The preparation method of sodium azulene sulfonate hemihydrate is the same as in Example 1.

[0057]10 g of sodium azulene sulfonate hemihydrate obtained after recrystallization was added to a water / dichloromethane mixed solvent with a volume ratio of 1:1, and fully stirred. The volume of water used was about 5% of the mass of sodium azulene sulfonate hemihydrate. times, after the crystal color changed from blue-black to blue, suction filtration, washing, and drying gave 11.3 g of sodium azulene sulfonate monohydrate with a yield of 91%.

[0058] Dried to constant weight, and tested the moisture result with a Karl Fischer moisture analyzer, the moisture content was 7.21%.

Embodiment 3

[0060] The preparation method of sodium azulene sulfonate hemihydrate is the same as in Example 1.

[0061] 10 g of sodium azulene sulfonate hemihydrate obtained after recrystallization was added to a water / ethyl acetate mixed solvent with a volume ratio of 1:1, and fully stirred. The volume of water used was about 5% of the mass of sodium azulene sulfonate hemihydrate. times, after the crystal color changed from blue-black to blue, filter with suction, wash and dry to obtain 5.2 g of sodium azulenesulfonate monohydrate with a yield of 51%.

[0062] Dry it to constant weight, and check the moisture result with a Karl Fischer moisture analyzer, and the moisture content is 7.33%.

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Abstract

The invention belongs to the field of chemical synthesis, and discloses a synthetic method for sodium gualenate monohydrate. The sodium gualenate monohydrate can be obtained in a way that sodium gualenate hemihydrate is added into a mixed solution of water and small polar organic solvent to be fully stirred and subjected to devitrification. The method is simple in operation, cost can be saved when the method is used for production, and operation personnel can easily master the synthetic process. Meanwhile, according to the method, single sodium gualenate monohydrate can be obtained, and purity is high. Waste liquid in the method is mainly an aqueous solution of sodium gualenate, petroleum ether can be subsequently recovered and used, and environment pollution is low.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a preparation method of sodium azulene sulfonate containing crystal water. Background technique [0002] Sodium azulene sulfonate, the active ingredient of chamomile flower, has strong anti-pepsin, anti-inflammatory, anti-bacterial, anti-allergic, and promoting mucosal metabolism. The mechanism of action: inhibits the release of histamine by local direct action; increases The synthesis of prostaglandin E2 in the mucosa can promote granulation formation and epithelial cell regeneration; and can reduce the activity of pepsin. Because of its high safety, it can be widely used in various pharmaceutical preparations, especially for the prevention and treatment of skin and oral diseases, and the effect is obvious. It can also be used to configure cosmetics, bath preparations, and soaps. [0003] Sodium azulene sulfonate, chemical name: 1,4-dimethyl-7-isopropyl azulene-3-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/25C07C303/32C07C303/44
CPCC07C303/32C07C303/44C07C309/25
Inventor 童巍邓书兰周静赵卿霍立茹李战
Owner NANJING GRITPHARMA CO LTD
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