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Method for preparing acetylated glucal

A technology of acetylated glucose and acetylation, applied in the field of preparation of acetylated gluculose, can solve the problems of rare reagents, cumbersome post-processing and high cost, and achieve the effect of reducing cost

Inactive Publication Date: 2006-07-19
朱书汉
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] The purpose of the present invention is to solve the shortcomings of cumbersome post-treatment, high cost and rare reagents in the preparation method of acetylated glucal sugar, and we provide a simple and effective synthesis method

Method used

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  • Method for preparing acetylated glucal
  • Method for preparing acetylated glucal
  • Method for preparing acetylated glucal

Examples

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Effect test

example 1

[0036] Example 1: Add 55kg D-glucose, 200L acetic anhydride, and catalytic amount of perchloric acid (10ml) to a 500L reactor, stir and dissolve, and control the reaction temperature at 15-45°C for 2 hours. At the end of the heat preservation, cool to below 5°C, pass in 7 cubic meters of hydrogen bromide, control the reaction temperature at 0-10°C and react for 2 hours. After the reaction is completed, pour it into a 2000L reactor (with 1000L of water), and then add 200L of chloroform , stirred for 30min, separated the chloroform, extracted the water layer once more with 100L of chloroform, combined the chloroform, then added 100L saturated aqueous solution of sodium bicarbonate to the chloroform, stirred for 30min, separated the chloroform, then added 300L of chloroform to the chloroform Saturated aqueous solution of sodium, stirred for 30 minutes, separated chloroform, transferred to a 500L dry kettle, added 25KG of anhydrous sodium sulfate, after 2 hours, filtered into a 500...

example 2

[0038] Example 2: Add 55kg D-glucose, 200L acetic anhydride, and catalytic amount of zinc chloride (50g) to a 500L reactor, stir and dissolve, and control the reaction temperature at 15-45°C for 2 hours. At the end of the heat preservation, cool to below 5°C, pass in 7 cubic meters of hydrogen bromide, control the reaction temperature at 0-10°C and react for 2 hours. After the reaction is completed, pour it into a 2000L reactor (with 1000L of water), and then add 200L of chloroform , stirred for 30min, separated the chloroform, extracted the water layer with 100L chloroform again, combined the chloroform, then added 100L saturated aqueous solution of sodium bicarbonate to the chloroform, stirred for 30min, separated the chloroform, then added 300L sodium chloride to the chloroform of saturated aqueous solution, stirred for 30min, separated chloroform, transferred to a 500L dry kettle, added 25KG of anhydrous sodium sulfate, and after 2 hours, filtered it into a 500L distillatio...

example 3

[0040] Example 3: Add 55kg of D-glucose, 200L of acetic anhydride, and 15ml of catalytic amount of p-toluenesulfonic acid to a 500L reactor, stir and dissolve, and control the reaction temperature at 15-45°C for 2 hours. At the end of the heat preservation, cool to below 5°C, add 90KG of phosphorus tribromide, then add 18KG of water, control the reaction temperature at 0-10°C for 2 hours, after the reaction is over, pour it into a 2000L reactor (with 1000L of water) , then add 200L of chloroform, stir for 30min, separate the chloroform, extract the water layer once more with 100L of chloroform, combine the chloroform, then add 100L of saturated aqueous solution of sodium bicarbonate to the chloroform, stir for 30min, separate the chloroform, and then add to the chloroform Add 300L of saturated aqueous solution of sodium chloride, stir for 30min, separate the chloroform, transfer to a 500L drying kettle, add 25KG of anhydrous sodium sulfate, after 2 hours, press filter into a 50...

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Abstract

The disclosed preparation method for acetylized glucal comprises: preparing the D-acetylized glucose catalyzed by acids (HClO4, H2SO4, ZnCl2, AlCl3, p-toluenesulfonic acid and methanesulfonic acid); without separation or purification, leading directly the product into HBr or equivalent (such as PBr3 and water) to obtain and then recrystallize the coarse 1-bromoacetyl glucose with one of ethyl ether, propyl ether and isopropyl ether; adding Zn, ZnCl2, methanol and Co-ion catalyst to prepare the coarse target; recrystallizing with alcohol for the refined product. This invention saves step and reduces cost.

Description

1. Technical field [0001] The invention relates to the technical field of organic chemistry, in particular to a method for preparing acetylated glucal sugar. 2. Background technology [0002] At present, there are many known methods for the preparation of acetylated glucal sugar, and more than a dozen kinds can be retrieved, and new processes are published every once in a while. There are mainly two methods: one is from the 2-position substitute Obtain the target object, such as: (1) Carbohydrate Research, 23(3), 369-77; 1972 [0003] [0004] This synthetic method is simple to operate, but the raw materials are expensive and rare. Such as: (2) Journal of Carbohydrate Chemistry, 6(2), 203-19; 1987 [0005] [0006] This synthesis method is simple to operate, but the raw materials are expensive and rare, and benzene is relatively toxic, so it is not suitable for use in pharmaceutical production. [0007] Another kind obtains the target object from the substituent of ...

Claims

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Application Information

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IPC IPC(8): C07H3/10C07H1/00
Inventor 朱书汉孙克俊
Owner 朱书汉
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