Isosorbide dimethyl ether synthesis
- Product Name:Isosorbide dimethyl ether
- CAS Number:5306-85-4
- Molecular formula:C8H14O4
- Molecular Weight:174.2
Isosorbide dimethyl ether is obtained from stock like D-sorbitol, which is mainly derived from the hydrogenation of D-glucose.
Isosorbide dimethyl has a low level of toxicity and is referred to as a green solvent due to its production from renewable/raw material.
The boiling point of this solvent is high.
lt is used as a substitute to dimethyl sulfoxide,and dimethylformamide-like solvents.
74-87-3
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652-67-5
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$5.00/25g
5306-85-4
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$7.00/5g
Yield:5306-85-4 74%
Reaction Conditions:
Stage #1:Isosorbide with sodium hydroxide in water at 60 - 90;Large scale;
Stage #2:methylene chloride in water at 80 - 90; under 3000.3 Torr;Large scale;
Steps:
2; 2.2-1-2.2-7 Preparation Example 2: Preparation of high purity dimethyl isosorbide using methyl chloride (MC method) and preparation of thin film distillation by-products
1,000 g of isosorbide was added to a pressurized reactor, heated to 60 to 70°C, stirred to melt transparently, and then 1,640 g of 50 wt% sodium hydroxide aqueous solution was slowly added while maintaining the reaction temperature at 80 to 90°C. After stirring for 0.5 to 1 hour, 1,209 g of methyl chloride was added while maintaining a reaction temperature of 80 to 90°C and an internal pressure of 4 bar or less. When the methyl chloride was no longer added, the temperature was maintained at 90° C. for 1 to 2 hours, and then cooled to room temperature. The salt produced by the reaction was removed through filtration, and the filtrate was neutralized in a pH range of 7 to 8 with 50% by weight of sodium hydroxide aqueous solution, and the salt produced by the neutralization reaction was removed again through filtration, and a rotary concentrator Water was removed from the neutralized filtrate by using, and residual salts were removed again through filtration to obtain about 834 g of reddish brown crude dimethyl isosorbide. The obtained crude dimethyl isosorbide showed a purity of about 87.2%.Subsequently, thin film distillation was performed on the obtained crude dimethyl isosorbide using a thin film distillation apparatus built in a condenser. Specifically, after setting the vacuum degree and temperature of the thin film distillation apparatus to 2.1 mbar and 72°C, respectively, thin film distillation was performed. % Yield) and about 75 g of thin film distillation by-products were obtained.At this time, the thin film distillation by-product is, based on a total of 100% by weight of the by-product, monomethyl isosorbide (MMI) 63.5% by weight, dimethyl isosorbide (DMI) 34.6% by weight, isosorbide 0.7% by weight and other impurities 1.2% by weight Included.
References:
Samyang Co., Ltd.;Im Jun-seop;Ryu Hun;Ryu Seung-hyeon KR102152693, 2020, B1 Location in patent:Paragraph 0041-0044; 0060-0074
