Method for synthesizing isosorbide dimethyl ether

A technology of isosorbide dimethyl ether and a synthesis method, which is applied to the synthesis of isosorbide dimethyl ether, and the etherification of isosorbide and methyl chloride to synthesize isosorbide dimethyl ether, can solve the problem of high production cost and achieve The effect of low vapor pressure, shortened reaction time, and reduced production cost

Active Publication Date: 2009-06-03
南京威尔药业科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, using isosorbide dimethyl ether as a solvent, the production cost is relatively high

Method used

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  • Method for synthesizing isosorbide dimethyl ether
  • Method for synthesizing isosorbide dimethyl ether
  • Method for synthesizing isosorbide dimethyl ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] In 1L stainless steel autoclave, add 300g molecular weight and be the polyethylene glycol of the methyl termination of 350, 200g (1.37mol) isosorbide, 164g (4.1mol) sodium hydroxide, 2g tetrabutyl ammonium bromide, stir Raise the temperature to 80°C, depressurize and dehydrate with a water pump, the vacuum gauge pressure is -0.095MPa, after the water is removed, feed in methyl chloride, control the pressure at 0.4MPa~0.5MPa, and measure the consumption of methyl chloride, when 208g of methyl chloride After consumption, lower the temperature to 60°C, neutralize to neutral with hydrochloric acid, remove the generated sodium chloride by filtration, conduct vacuum distillation on the filtrate, collect 92°C-93°C / 2mmHg fractions, and obtain 219g of isosorbide dimethyl ether, Yield 92%. 290 g of polyether was recovered.

Embodiment 2

[0042] In 1L stainless steel autoclave, add 300g molecular weight and be the monomethoxy polyethylene glycol of 350, 200g (1.37mol) isosorbide, 216g (5.4mol) sodium hydroxide, 2g tetrabutyl ammonium bromide, stir Raise the temperature to 80°C, depressurize and dehydrate with a water pump, and the vacuum gauge pressure is -0.095MPa. After the water is removed, introduce methyl chloride, control the pressure at 0.4MPa-0.5MPa, and measure the consumption of methyl chloride. When 273g of methyl chloride After consumption, lower the temperature to 60°C, neutralize to neutral with hydrochloric acid, remove the generated sodium chloride by filtration, conduct vacuum distillation on the filtrate, collect fractions at 92°C to 93°C / 2mmHg to obtain 216g of isosorbide dimethyl ether, Yield 91%. 298 g of polyether was recovered.

Embodiment 3

[0044] The reaction conditions are the same as those in Example 1, 250 g of recycled polyether was used as the solvent, and 50 g of fresh polyether was added to obtain 226.5 g of isosorbide dimethyl ether with a yield of 95%.

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Abstract

A method for synthesizing isosorbide dimethyl ether comprises the following steps: (1) adding solvent, isosorbide, alkali and phase transfer catalyst in a reaction vessel; (2) stirring and raising the temperature to 80 to 100 DEG C, reducing the pressure until the gauge pressure is minus 0.095 MPa, and dewatering; (3) leading into chloromethane under the condition of the phase transfer catalyst, and complete the etherification reaction with the pressure 0.1 to 1.0 MPa and the temperature 50 to 90 DEG C; (4) carrying out acid neutralization; (5) filtering and desalting; (6) and carrying out reduced pressure distillation, and collecting fraction with the temperature of 92 to 93 DEG C to get isosorbide dimethyl ether and recovering the solvent. The solvent adopts low molecular polyether with alkyl sealing the ends, in the formulae, R1 and R2 are hydrogen atoms or alkyl; the adopted alkyl comprises 1 to 15 carbon atoms; R3 and R4 are hydrogen atoms or methyl, or other lower alkyl; and m plus n is an integer between 4 to 15. The invention realizes zero discharge, reduces cost and increases production efficiency.

Description

technical field [0001] The invention relates to a synthesis method, in particular to a synthesis method of isosorbide dimethyl ether, in particular to a method for synthesizing isosorbide dimethyl ether by etherification of isosorbide and methyl chloride in the presence of a phase transfer catalyst. The etherification reaction is completed in a system with low molecular weight polyether as the medium. technical background [0002] Dimethyl isosorbide, also known as dimethyl isosorbide (DMI), 1,4:3,6-dianhydro-2,5-di-oxo-methyl-D-glucitol, 1,4 : 3,6-dianhydrosorbitol 2,5-dimethyl ether, etc. [0003] Isosorbide dimethyl ether is a colorless oily liquid, stable under neutral conditions, hygroscopic, miscible with many organic solvents, and often used as a solvent. DMI can promote the penetration of active ingredients into the epidermis of the skin and give full play to the effectiveness of active ingredients. Mainly used in medicine and cosmetics. [0004] Isosorbide dimet...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/04
Inventor 高正松贾建国沈德渊周霞娟
Owner 南京威尔药业科技有限公司
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