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Method for synthesizing glassine by one-pot method

A technology for boson and substance, which is applied to the field of one-pot synthesis of boson, can solve the problems of complex catalyst structure, difficult preparation and high production cost of the synthesis process, and achieve the effects of low price, easy availability and simple operation.

Pending Publication Date: 2021-07-20
海南夸克科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The structure of the catalyst used in this method is relatively complex and not easy to obtain, and the production cost of the overall synthesis process is relatively high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 500 g of ethanol, 30 g (0.2 mol) of xylose, 0.17 g (2 mmol) of sodium bicarbonate, and 26 g (0.2 mol) of ethyl acetoacetate into a 1000 mL reaction flask in sequence, stir and raise the temperature to 60 ° C, and continue the reaction for 1 h. It was detected by TLC that xylose basically disappeared (GF254 silica gel plate, developing solvent: dichloromethane:methanol=4:1, 20% sulfuric acid ethanol solution for color development). Then 11.3 g (0.3 mol) of sodium borohydride was added dropwise at 0°C, stirred evenly and reacted at 50°C for 24 hours, then slowly added 2N hydrochloric acid dropwise to adjust the pH to neutral, and then extracted and separated with ethyl acetate. The organic layer was collected and spin-dried to obtain 32.8 g of a light yellow oily substance, ie Bosene, with a yield of 85.3%.

[0022] 1 H NMR(DMSO)δ=4.30(brs,4H),3.75(m,1H),3.65(m,1H),3.25(m,1H),3.14(m,1H),2.96(m,2H),2.83 (m,1H),1.73(m,1H),1.45(m,1H),1.03(d,3H).

Embodiment 2

[0024] Add 500g of n-butanol, 30g (0.2mol) of xylose, 0.4g (10mmol) of sodium hydroxide, and 43.2g (0.3mol) of isopropyl acetoacetate into a 1000mL reaction flask in sequence, stir and raise the temperature to 60°C, and continue the reaction After 1 h, the reaction solution was detected by TLC until the xylose basically disappeared (GF254 silica gel plate, developer: dichloromethane:methanol=4:1, 20% sulfuric acid ethanol solution for color development). Then 21.6 g (0.4 mol) of potassium borohydride was added dropwise at 0°C, stirred evenly, and reacted at 100°C for 8 hours, then quenched with 2N hydrochloric acid, filtered, and the filtrate was concentrated to obtain 33.2 g of light yellow oil, i.e. glass Chromogen, the yield is 86.4%.

Embodiment 3

[0026] Add 500g of isopropanol, 36g (0.2mol) of xylose, 0.34g (6mmol) of potassium hydroxide, and 38g (0.24mol) of isobutyl acetoacetate into a 1000mL reaction flask in sequence, stir and raise the temperature to 60°C, and continue the reaction for 1h , the reaction solution was detected by TLC until the xylose basically disappeared (GF254 silica gel plate, the developer was dichloromethane:methanol=4:1, 20% sulfuric acid ethanol solution for color development). Then 13.6g (0.36mol) of sodium borohydride was added dropwise at 0°C, stirred evenly and reacted at 80°C for 12h, quenched with 2N hydrochloric acid, spin-dried, dissolved in 500ml of ethanol, filtered, and the filtrate was concentrated to obtain 33.1 g Pale yellow oil, that is, Boseine, the yield is 86.1%.

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Abstract

The invention discloses a method for synthesizing a bose by a one-pot method, which comprises the following step of: synthesizing the bose by the one-pot method under the action of a catalyst and a reducing agent by taking xylose and acetoacetate substances as raw materials in the presence of an organic solvent. The method has the advantages of easily available catalyst and reducing agent, low cost and high yield, and is suitable for industrial production.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a method for synthesizing Boseine by a one-pot method. Background technique [0002] Boseine, whose scientific name is hydroxypropyltetrahydropyranotriol, is a bioactive ingredient used in cosmetics developed by L'Oreal in 2006, which can promote the production and construction of proteoglycans in the extracellular matrix , and absorb water, make the matrix gel, increase the firmness of cells and skin; it can also stimulate aging cells, promote the regeneration of damaged tissues, help maintain the elasticity of the dermis, and prevent skin aging. Studies have shown that Boseine is easy to biodegrade, does not accumulate in organisms, and has no toxicity. This characteristic further increases the application of Boseine in the fields of biology, medicine, and cosmetics. [0003] As for the synthesis method of Boseine, there are only some chemical synthesis literature reports in C...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D309/10
CPCC07D309/10
Inventor 韩津蓝艳
Owner 海南夸克科技有限公司