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After-treatment method of benzylation reaction product

A reaction product, a technology of benzylation, applied in chemical instruments and methods, organic chemistry, sugar derivatives, etc., can solve the problems of complicated operation, low purity and yield of benzylation reaction products, etc.

Active Publication Date: 2015-03-11
SHANDONG SHENGQUAN NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The inventor used the post-treatment method of the reaction solution after the above-mentioned benzylation reaction was completed to the above-mentioned benzylation reaction disclosed by the Chinese patent No. CN03157827.6. The experimental results showed that the obtained benzylation reaction product The purity and yield are low, and the reaction solution needs to be repeatedly extracted and chromatographic column purified, and the operation is cumbersome

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Dissolve 1 mol of methyl-1-ethylthio-β-L-fucoside completely with 14 mol of DMF while stirring, then start to heat up at 5°C, and slowly add 6 mol of NaH, after the temperature rises to 40°C Start to add 3 mol of benzyl chloride dropwise to it, and keep the temperature between 40°C and 50°C; Ethylthio-β-L-fucoside reacted completely.

[0054]After the reaction is complete, slowly add water at 20°C to quench the benzylation reaction until no bubbles are generated; after quenching, filter the obtained reaction solution, add 10mol deionized water to the obtained filtrate, and then Carry out vacuum distillation at 50°C with a vacuum degree of 0.09MPa, and repeat the vacuum distillation twice; then add 50mol deionized water and 4mol methylene chloride to the obtained vacuum distillation product, stir and extract for 5 minutes, and repeat the extraction 2 times to obtain the organic phase extraction product; dry the obtained organic phase extraction product with sodium sulfa...

Embodiment 2

[0061] Dissolve 1 mol of methyl-1-ethylthio-β-L-fucoside completely with 15 mol of DMF while stirring, then start to heat up at 20°C and slowly add 6.3 mol of NaH, and keep the temperature below 30°C ℃, the temperature was raised to 40℃, and 3.2mol benzyl chloride was added dropwise therein, and the temperature was kept between 40℃~50℃ during the dropwise addition; after the dropwise addition, the temperature was kept at 20℃ °C for 12 hours. And the reaction solution is tested by TLC to judge whether the raw material methyl-1-ethylthio-β-L-fucoside has reacted completely.

[0062] After the reaction was complete, water was slowly added to the reaction system, and the reaction was quenched at 25° C. until no more bubbles were generated. After the quenching is completed, filter the reaction solution, add 25mol deionized water to the filtrate, then heat and distill under reduced pressure at 45°C and a vacuum of 0.1MPa, repeat the reduced-pressure distillation twice; Add 60 mol ...

Embodiment 3

[0069] Dissolve 1 mol of 1-O-tert-butyl-β-L-arabinoside completely with 14.5 mol of DMF under stirring conditions, then start to heat up at 20°C and slowly add 6.1 mol of NaH to it, and the temperature does not exceed 30 In the case of ℃, the addition is complete, after the temperature is raised to 40 ℃, 3.1 mol benzyl chloride is added dropwise to it, and the temperature is kept between 40 ℃ and 50 ℃ during the dropwise addition; after the dropwise addition, the temperature is kept at 20 ℃ The reaction was carried out for 12 hours. And the reaction solution was tested by TLC to judge whether the reaction of the raw material 1-O-tert-butyl-β-L-arabinoside was complete.

[0070] After the reaction is complete, slowly add water to the reaction system, and quench the reaction at 30°C until no more bubbles are produced; after the quenching is completed, filter the reaction solution, add 25mol deionized water to the filtrate, and then Heating and vacuum distillation at 45°C and a ...

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Abstract

The invention provides an after-treatment method of a benzylation reaction product. The after-treatment method includes the following steps of (a), adding water into a reaction solution which finishes a benzylation reaction, and subjecting a mixture to distillation to obtain a distillation product, wherein the temperature of the distillation can not exceed 60 DEG C, and the reaction solution comprises N, N-dimethyl formamide, sodium hydride, the benzylation reaction product, a benzylation reagent and a benzylation by-product; (b), subjecting the distillation product obtained from the step (a) to extraction to obtain an organic phase extraction product; and (c), sequentially subjecting the organic phase extraction product obtained from the step (b) to distillation and purification to obtain the benzylation reaction product. According to the after-treatment method of the benzylation reaction product, the amount of the N, N- dimethyl formamide and the by-product of benzyl alcohol is reduced, the influence on the product during the extraction and the purification is reduced, the influence is caused by a large amount of the N, N-dimethyl formamide and the benzyl alcohol, and the obtained benzylation reaction product is high in yield and purity.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for post-processing a benzylation reaction product. Background technique [0002] Benzylation is a reaction to introduce benzyl groups into organic compound molecules, which has a wide range of applications in organic synthesis. For example, Zhao Fengge and others have synthesized a large molecular weight benzyl substituted product through the benzylation reaction of biphenyl, which successfully reduces the freezing point of the heat transfer oil (Zhao Fengge, Dong Huiru, Liu Guowen. Synthesis of high temperature heat transfer oil by biphenyl benzylation reaction Research. Journal of Beijing University of Chemical Technology (Natural Science Edition), 2003,30(1):76~79.); Wu Yun et al. used the benzylation reaction of benzene to synthesize diphenylmethane (Wu Yun, Sagala, Zhang Yu, Zhao Histogram.CuCl 2 / clay-sa 01 Catalytic benzylation of benzene to diphenyl...

Claims

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Application Information

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IPC IPC(8): C07H15/18C07H1/06
Inventor 江成真刘顶
Owner SHANDONG SHENGQUAN NEW MATERIALS CO LTD
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