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A kind of production technology of VC ethyl ether

A production process and technology of ethyl ether, applied in the field of production technology of Vc ethyl ether, can solve the problems of inability to ensure the purity of Vc ethyl ether finished product, high equipment and control costs, and many times of material transfer, etc. The effect of waste treatment costs, reduced equipment and control costs, and reduced process time

Active Publication Date: 2022-05-06
ZHEJIANG TOP MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This patent optimizes the traditional three-step method, and replaces acetone with acetone dimethyl acetal, and produces methanol after the reaction, which is easy to remove and avoids affecting the purity of the product; moreover, DMSO is effectively recovered to increase the yield; However, this method still does not solve the problem of by-products in the 3-position substitution reaction process, so it cannot ensure that the Vc ethyl ether finished product has good purity, and there are many steps, many material transfer times, and high equipment and control costs.

Method used

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  • A kind of production technology of VC ethyl ether
  • A kind of production technology of VC ethyl ether

Examples

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Embodiment 1

[0034] A production process of Vc ethyl ether, adopting the following synthetic route: taking vitamin C as a starting material, through acetonylidene protection, etherification and hydrolysis deprotection, to obtain Vc ethyl ether; the production process specifically includes the following steps :

[0035] S1. Condensation: Add 255-265kg of vitamin C, 200-250kg of acetone dimethyl acetal, 800-850kg of DMSO and 4.5-5.5kg of catalyst into the reaction tank for condensation reaction. The catalyst is p-toluenesulfonic acid Or the pyridinium salt of p-toluenesulfonic acid, and the molar ratio of catalyst to acetone dimethyl acetal is 1: (65-85), the reaction temperature is controlled at 25-35°C, and the reaction time is 2.5-4.5h; after the reaction is completed, put it in the reaction tank Add 4.5-5.5kg of sodium bicarbonate to neutralize the condensation product, and then separate methanol and residual acetone dimethyl acetal by distillation;

[0036] S2. Etherification: Add 200-...

Embodiment 2

[0040] This embodiment provides a production process of Vc ethyl ether, which is a further optimization of the scheme of Example 1. The production process specifically includes the following steps:

[0041]S1. Condensation: 260kg of vitamin C, 215.2 of acetone dimethyl acetal, 813kg of DMSO and 5.1kg of p-toluenesulfonic acid are added to the reaction tank for condensation reaction, the reaction temperature is controlled at 28.0°C, and the reaction time is 3.5h; the reaction is over Add 4.96kg of sodium bicarbonate and the condensation product in the reaction tank to neutralize, then separate methanol and residual acetone dimethyl acetal through distillation;

[0042] S2. Etherification: Add 210kg of sodium bicarbonate and 4.0kg of water to the condensation product after distillation, mix well, then dissolve 255kg of bromoethane in DMSO 0.5 times its volume in advance to obtain a mixed solution, and then Add the mixed solution dropwise to the condensation product for etherific...

Embodiment 3

[0046] A production process of Vc ethyl ether is basically the same as in Example 2, except that in step S4, no isopropyl acetate is added after cooling and crystallization, and the crystals are collected by centrifugation directly. The finished product yield of Vc ethyl ether was 65.1%, and the purity was 99.3%. When no isopropyl acetate was added, the yield of Vc ethyl ether decreased, and the purity had little influence.

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Abstract

The invention belongs to the technical field of chemical synthesis, and specifically discloses a production process of Vc ethyl ether. The Vc ethyl ether adopts the following synthesis route: taking vitamin C as a starting material, acetonide protection, etherification and hydrolysis deprotection, Vc ethyl ether is obtained; the production process includes condensation, etherification, hydrolysis and refining steps. The present invention replaces acetone with acetone dimethyl acetal, which avoids the problem of Vc ethyl ether production rate decline caused by acetone in the traditional three-step method; reduces the production of by-products in the etherification process by controlling the addition of bromoethane, and passes brine- The extraction system of toluene removes DMSO, effectively improving the product purity; according to the process of the present invention to prepare Vc ethyl ether, the yield can reach more than 65%, and the purity of the finished product can reach more than 99%. In addition, the invention has a simple process, does not need frequent material transfer, and has high efficiency and low cost.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a production process of Vc ethyl ether. Background technique [0002] Vitamin C is difficult to be absorbed by the skin, and is easily oxidized to cause discoloration. As a whitening agent, its application in cosmetics is limited. Vc ethyl ether is a new lipophilic and benign vitamin C derivative with the following structural formula: [0003] [0004] It has good stability and is easy to penetrate the stratum corneum of the skin and enter the dermis. After entering the skin, it is easily decomposed by biological enzymes to exert the biological effects of vitamin C, thereby improving its bioavailability, so it is widely used as a cosmetic product. Anti-aging agent and whitening agent. [0005] There are one-step and three-step methods for the synthesis of Vc ethyl ether. The one-step method is to directly use vitamin C and ethyl methanesulfonate or su...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/62A61Q19/08A61Q19/02
CPCC07D307/62A61Q19/08A61Q19/02
Inventor 谢再法姚凤鸣郭锋燕
Owner ZHEJIANG TOP MEDICINE
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