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One-pot method for preparing dimethyl carbonate under low-pressure conditions

A technology of dimethyl carbonate and conditions, applied in the field of organic synthesis and catalysis, can solve the problems of large amount of catalyst, difficult catalyst preparation, and high reaction pressure of the catalytic system, and achieves the effects of mild conditions, easy industrial production, and reduced production cost.

Inactive Publication Date: 2019-12-13
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the reported catalytic systems have shortcomings such as high reaction pressure, large amount of catalyst, and difficulty in catalyst preparation (Green Chemistry, 2003, 5, 71; Industrial & Engineering Chemistry Research, 2003, 42, 3865; Catalysis Letters, 2010, 141 , 339)

Method used

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  • One-pot method for preparing dimethyl carbonate under low-pressure conditions
  • One-pot method for preparing dimethyl carbonate under low-pressure conditions
  • One-pot method for preparing dimethyl carbonate under low-pressure conditions

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Embodiment 1

[0020] The preparation of embodiment 1 dimethyl carbonate

[0021] Na 2 CO 3 (0.25 mmol), choline bromide (0.1 mmol), propylene oxide (5 mmol), and methanol (90 mmol) were added to the high-pressure reaction kettle, and then carbon dioxide was introduced to make the system pressure reach 0.5 MPa, and the reaction was performed under magnetic stirring at 140 °C. After 6 hours, after the end of the reaction, quantitative analysis by gas chromatography internal standard method showed that the yield of dimethyl carbonate was 64%.

Embodiment 2

[0022] The preparation of embodiment 2 dimethyl carbonate

[0023] K 2 CO 3 (0.25 mmol), choline bromide (0.05 mmol), propylene oxide (5 mmol), and methanol (90 mmol) were added to the high-pressure reactor, and then carbon dioxide was introduced to make the system pressure reach 0.5 MPa, and the reaction was performed under magnetic stirring at 140 °C. After 6 hours, after the reaction was finished, quantitative analysis by gas chromatography internal standard method showed that the yield of dimethyl carbonate was 58%.

Embodiment 3

[0024] The preparation of embodiment 3 dimethyl carbonate

[0025] Cs in turn 2 CO 3 (0.25 mmol), choline bromide (0.05 mmol), propylene oxide (5 mmol), and methanol (90 mmol) were added to the high-pressure reaction kettle, and then carbon dioxide was introduced to make the system pressure reach 0.5 MPa, and the reaction was performed under magnetic stirring at 140 °C. After 6 hours, after the end of the reaction, quantitative analysis by gas chromatography internal standard method showed that the yield of dimethyl carbonate was 57%.

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Abstract

The invention discloses a one-pot method for preparing dimethyl carbonate under low-pressure conditions, and belongs to the field of organic synthesis and catalysis. According to the method, carbon dioxide, an epoxy compound and methanol are used as raw materials, a carbonate and choline bromide are used as a two-component catalyst, and no solvent is required to be added additionally to prepare dimethyl carbonate. Under optimized reaction conditions, the yield of dimethyl carbonate taking propylene oxide as a raw material is 64%, and the yield of dimethyl carbonate is still 56% after a catalytic system is repeatedly used for three times. When ethylene oxide is used as a raw material, the yield of dimethyl carbonate can reach 87%. The method for synthesizing dimethyl carbonate has the advantages of cheap and easily available catalyst, mild reaction conditions, simple operation and high atom economy, the catalyst can be repeatedly used, and an excellent system for preparing dimethyl carbonate is obtained.

Description

technical field [0001] The invention relates to a method for preparing dimethyl carbonate in one pot by catalyzing carbon dioxide, epoxide and methanol under mild conditions with a two-component catalyst, which belongs to the field of organic synthesis and catalysis. Background technique [0002] Dimethyl carbonate is an important organic synthesis intermediate, which has been widely used as methylating reagent, carbonylating reagent, excellent solvent and gasoline additive (Organic letters, 2001, 3, 4279; Accounts of Chemical Research, 2002, 35, 706 ; Journal of Organic Chemistry, 2003, 68, 1954). [0003] The one-pot synthesis of dimethyl carbonate from carbon dioxide, epoxide and methanol is one of the effective methods for preparing dimethyl carbonate (Green Chemistry, 2003, 5, 71; Applied Catalysis A: General, 2004, 263,179; Catalysis Letters, 2008 , 128, 459). The advantage of this method is that after carbon dioxide and epoxide cycloaddition, there is no need to sep...

Claims

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Application Information

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IPC IPC(8): C07C68/04C07C69/96B01J31/02
CPCB01J31/0239B01J31/0271B01J2231/49C07C68/04C07C69/96Y02P20/141
Inventor 刘春刘凯
Owner DALIAN UNIV OF TECH