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Synthesizing method for whitening agent raw materials

A synthesis method and whitening agent technology, applied in the field of synthesis of vitamin C ethyl ether, can solve the problems of no significant improvement in yield and purity, and achieve the effects of easy-to-obtain raw materials, simple process, and high yield

Inactive Publication Date: 2017-04-19
BEIJING HUAXIN LONGYUE TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] The collection of raw materials and the control of temperature in the production process in the above production processes have all met the cost control and safety requirements, but the yield and purity issues have not been significantly improved, and there is no solution to the core issues such as yield and purity. come up with effective solutions

Method used

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  • Synthesizing method for whitening agent raw materials
  • Synthesizing method for whitening agent raw materials

Examples

Experimental program
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Effect test

Embodiment 1

[0045] Add 0.1mol ascorbic acid (17.6g), 2mol acetone (116.2g), 0.006mol anhydrous copper sulfate (0.96g) to a 1L reactor successively, stir, react in a water bath at 30°C for 15h, and analyze by TLC during the reaction The chromatographic board is used for monitoring. After the reaction of ascorbic acid is completed, the obtained reaction solution is suction-filtered while it is hot, and the copper sulfate with crystal water is filtered out to obtain an acetone solution with 5,6-O-isopropylidene-L-ascorbic acid.

[0046] Because anhydrous copper sulfate is used as the catalyst, it will not cause the reaction to obtain a relatively acidic solution, so directly add 0.1mol (13.8g) potassium carbonate to the above solution, protect it with nitrogen, and react at about 60°C for 0.5h, then directly Add 0.1mol (10.9g) bromoethane, continue to react for 1-2h, insoluble potassium bromide is formed, after filtering, 3-O-ethane-5,6-O-isopropylidene-L- Acetone solution of ascorbic acid. ...

Embodiment 2

[0050] Add 0.1mol ascorbic acid (17.6g), 2mol acetone (116.2g), 0.006mol anhydrous copper sulfate (0.96g) to a 1L reactor successively, stir, react in a water bath at 30°C for 15h, and analyze by TLC during the reaction The chromatographic board is used for monitoring. After the reaction of ascorbic acid is completed, the obtained reaction solution is suction-filtered while it is hot, and the copper sulfate with crystal water is filtered out to obtain an acetone solution with 5,6-O-isopropylidene-L-ascorbic acid.

[0051] Because anhydrous copper sulfate is used as the catalyst, it will not cause the reaction to obtain a relatively acidic solution, so directly add 0.1mol (13.8g) potassium carbonate to the above solution, protect it with nitrogen, and react at about 60°C for 0.5h, then directly Add 0.1mol (10.9g) bromoethane, continue to react for 1-2h, insoluble potassium bromide is formed, after filtering, 3-O-ethane-5,6-O-isopropylidene-L- Acetone solution of ascorbic acid. ...

Embodiment 3

[0055] Add 0.1mol ascorbic acid (17.6g), 2mol acetone (116.2g), 0.006mol anhydrous copper sulfate (0.96g) to a 1L reactor successively, stir, react in a water bath at 30°C for 15h, and analyze by TLC during the reaction The chromatographic board is used for monitoring. After the reaction of ascorbic acid is completed, the obtained reaction solution is suction-filtered while it is hot, and the copper sulfate with crystal water is filtered out to obtain an acetone solution with 5,6-O-isopropylidene-L-ascorbic acid.

[0056] Because anhydrous copper sulfate is used as the catalyst, it will not cause the reaction to obtain a relatively acidic solution, so directly add 0.1mol (13.8g) potassium carbonate to the above solution, protect it with nitrogen, and react at about 60°C for 0.5h, then directly Add 0.1mol (10.9g) bromoethane, continue to react for 1-2h, insoluble potassium bromide is formed, after filtering, 3-O-ethane-5,6-O-isopropylidene-L- Acetone solution of ascorbic acid. ...

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Abstract

Vitamin C ethyl ether is an oleophylic and hydrophilic amphiprotic vitamin C ramification. The vitamin C and acetone are raw materials, anhydrous cupric sulfate serves as a catalyst for the reaction to synthesize 5,6-O-isopropylidene-L-ascorbic acid (IAA for short); IAA and bromoethane (CH3CH2Br) serve as raw materials, and under the existence of acetone and potassium carbonate, 3-O-ethane-5,6-O-isopropylidene-L-ascorbic acid is synthesized; hydrochloric acid is added to remove a protecting group; and superior product vitamin C ethyl ether is obtained through recrystallization. Compared with a traditional synthetic method, the technology is simple and convenient to conduct, raw materials are easy to obtain, the raw materials are bulk chemical raw materials, the cost is low, the yield is high, and industrial popularization is easy.

Description

technical field [0001] The invention relates to a method for synthesizing whitening agent raw materials, mainly for the synthesis method of vitamin C ethyl ether. Background technique [0002] Vitamin C ethyl ether is a lipophilic amphoteric vitamin C derivative, which not only makes it extremely convenient to use in the formula, but also makes it easier to penetrate the stratum corneum and enter the dermis, and it is easy to enter the skin after entering the skin. It is decomposed by biological enzymes to play the role of vitamin C, thereby improving its bioavailability, effectively whitening and removing spots, improving dull and dull skin, and giving skin elasticity. [0003] Chemical name: 3-O-ethyl ascorbic acid [0004] INCI name: 3-o-ETHYL ASCORBIC ACID [0005] Molecular formula: C 8 h 12 o 6 [0006] [0007] Chemical formula of vitamin C ethyl ether [0008] As a new type of whitening agent, vitamin C ethyl ether is more and more favored by the cosmetics ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/62
CPCY02P20/55C07D307/62
Inventor 裴双秀张霞
Owner BEIJING HUAXIN LONGYUE TECH CO LTD
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