Sodium stearyl fumarate auxiliary material and preparation method thereof

A technology of sodium stearyl fumarate and auxiliary materials is applied in directions such as carboxylate preparation, chemical instruments and methods, preparation of organic compounds, etc., and can solve problems such as increasing production cost and time, unfavorable industrialized production, and tedious synthesis process, etc. To achieve the effect of simplifying the preparation process and post-processing steps, reducing the residual solvent components, and improving the total yield

Active Publication Date: 2018-09-28
苏州东南药业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the prior art, stearyl alcohol and maleic anhydride are usually used as raw materials to prepare hard sodium fumarate, but in the preparation process, various solid intermediate products often need to be prepared successively, which not only leads to many prepa

Method used

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  • Sodium stearyl fumarate auxiliary material and preparation method thereof
  • Sodium stearyl fumarate auxiliary material and preparation method thereof
  • Sodium stearyl fumarate auxiliary material and preparation method thereof

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preparation example Construction

[0028] Such as figure 1 Shown, the invention provides a kind of preparation method of sodium stearyl fumarate auxiliary material, comprises the following steps:

[0029] S1. Mix maleic anhydride, stearyl alcohol and a reaction solvent, and perform a ring-opening reaction at a temperature of 80° C. or above;

[0030] S2, adding a conversion agent to the reaction system to perform a conversion reaction;

[0031] S3, cooling down to 40-50°C, adding a sodium-containing alkali solution dropwise to the reaction system, cooling down and crystallizing after the stirring reaction is completed, and obtaining crude sodium stearyl fumarate;

[0032] S4. Refining the crude sodium stearyl fumarate to obtain a sodium stearyl fumarate product.

[0033] Following is the process route of the present invention:

[0034]

[0035] In one embodiment, in step S1, the present invention uses maleic anhydride and stearyl alcohol as raw materials, puts them in a reaction solvent, raises the temper...

Embodiment 1

[0044] The preparation of embodiment 1 sodium stearyl fumarate

[0045] Add 103.0g of maleic anhydride, 270.00g of stearyl alcohol and 1000mL of toluene into the reaction vessel, and heat to 85°C for 12 hours to react. To the reaction system, add 10% hydrochloric acid / thiourea solution (the mass ratio of hydrochloric acid and thiourea is 1:1), react at 80°C for 16 hours, and detect by gas phase: Intermediate II / Intermediate I is 99.5% . Subsequently, the temperature was lowered to 45°C, and 320 mL of an aqueous solution containing 51.5 g of sodium hydroxide was added dropwise to the reaction system. After 1 hour, the dropwise addition was completed. Stirring was continued for 1 hour, cooled to room temperature, stirred for 1 hour, and filtered to obtain stearyl fumar Crude Sodium Acid. Add the crude product and 2Kg ethanol into a reaction vessel, raise the temperature to 50°C, and beat at this temperature for 7 hours, cool down to 20°C, filter, wash with ethanol, and dry t...

Embodiment 2

[0046] The preparation of embodiment 2 sodium stearyl fumarate

[0047] 123.5 g of maleic anhydride, 324.06 g of stearyl alcohol and 1200 mL of cyclohexane were added to the reaction vessel, and the mixture was heated to 90° C. for 15 hours to react. To the reaction system, add 8% hydrochloric acid / thiourea solution (the mass ratio of hydrochloric acid and thiourea is 1:1), and react at 72° C. for 10 hours. Subsequently, the temperature was lowered to 48°C, and 650 mL of an aqueous solution containing 49.5 g of sodium hydroxide was added dropwise to the reaction system. After 1 hour, the dropwise addition was completed. Stirring was continued for 1 hour, cooled to room temperature, stirred for 2 hours, and filtered to obtain stearyl fumar Crude Sodium Acid. Add the crude product and 4.2Kg ethanol into a reaction vessel, raise the temperature to 50°C, and beat for 5 hours at this temperature, cool down to 22°C, filter, wash with ethanol, and vacuum freeze-dry the obtained so...

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Abstract

The invention provides a sodium stearyl fumarate auxiliary material and a preparation method thereof. The preparation method comprises the following steps: S1, mixing maleic anhydride, octadecanol anda reaction solvent, heating, and carrying out a ring-opening reaction; S2, adding a converting agent to carry out a conversion reaction; S3, cooling, dropping a sodium-containing alkali solution, stirring, and cooling to separate a crystal after the reaction is completed so as to obtain a crude product; S4, carrying out refining treatment, so as to obtain a sodium stearyl fumarate product. Sodiumstearyl fumarate is prepared by using a one-pot method, middle products do not need to be separated, preparation processes and aftertreatment steps can be greatly simplified, and reaction conditionsare gentle; moreover, the total yield is remarkably increased, the purity is remarkably improved, and the sodium stearyl fumarate auxiliary material is suitable for being used as a medicine and food auxiliary material and is applicable to industrial production.

Description

technical field [0001] The invention belongs to the technical field of auxiliary material preparation, and in particular relates to a sodium stearyl fumarate auxiliary material and a preparation method thereof. Background technique [0002] Sodium stearyl fumarate (C 22 h 39 NaO 4 ) is a widely used and important pharmaceutical and food excipient. During the metabolism of sodium stearyl fumarate in animals, most of it can be absorbed and hydrolyzed to produce stearyl alcohol and stearic acid, and a small part can be directly and quickly metabolized, which is non-toxic and non-irritating. In the field of pharmaceuticals, sodium stearyl fumarate is added to pharmaceutical preparations, which can be used as a lubricant for tablets and capsules, and can also form a protective film in effervescent tablets, which can solve the problem of stearate lubricants. Existing problems, and can improve drug disintegration, promote the effect of drug stripping. In the field of food, FDA...

Claims

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Application Information

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IPC IPC(8): C07C69/60C07C67/08C07C67/333C07C67/30C07C67/48
CPCC07C67/08C07C67/30C07C67/333C07C67/48C07C69/60
Inventor 刘海东吉民王冬冬宗玺胡海燕张影
Owner 苏州东南药业股份有限公司
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