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N,N-dimethylformamide dimethyl acetal synthesis method

A technology of dimethylformamide and dimethyl acetal, which is applied in chemical instruments and methods, preparation of amino hydroxyl compounds, preparation of organic compounds, etc., can solve problems such as harsh reaction conditions, achieve fast dissolution, reduce costs, The effect of mild reaction conditions

Active Publication Date: 2016-11-09
HENAN CHEM IND RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

People such as Pan Yi adopt liquid sodium methylate, distill methanol, then add sherwood oil, productive rate improves to some extent, but still adopt sherwood oil as solvent in the second step reaction, need to control temperature below 0 ℃ during reaction, and reaction condition is harsh ( Optimization of the preparation process of N,N-dimethylformamide dimethyl acetal, Fine Chemical Intermediates, 2008)

Method used

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Embodiment 1

[0030] A kind of synthetic method of N,N-dimethylformamide dimethyl acetal, comprises the following steps:

[0031] (1) Heat N,N-dimethylformamide to 60°C, keep warm, add dimethyl sulfate dropwise, react for 5 hours after the dropwise addition, and obtain an imine complex, cool to room temperature, and set aside; among them, N , the mol ratio of N-dimethylformamide and dimethyl sulfate is 1:1;

[0032] (2) Add solid sodium methoxide to isododecane, mechanically stir and disperse, adjust the temperature to 20°C, keep warm, add the imine complex dropwise, react for 3 hours after the dropwise addition, filter, and fractionate the filtrate under normal pressure , collecting fractions at 105-108°C to obtain N,N-dimethylformamide dimethyl acetal with a yield of 72.6% and a purity of 97%; wherein the molar ratio of sodium methoxide to imine complex is 1: 1;

[0033] In step (2), the ratio of solid sodium methylate and isododecane is that every 1mol of sodium methylate is dispersed ...

Embodiment 2

[0035] A kind of synthetic method of N,N-dimethylformamide dimethyl acetal, comprises the following steps:

[0036] (1) Heat N,N-dimethylformamide to 70°C, keep warm, add dimethyl sulfate dropwise, and react for 4 hours after the dropwise addition to obtain an imine complex, cool to room temperature, and set aside; among them, N , the mol ratio of N-dimethylformamide and dimethyl sulfate is 1:1;

[0037] (2) Add solid sodium methoxide to 200# solvent oil, ultrasonically disperse, adjust the temperature to 25°C, keep warm, add the imine complex dropwise, react for 2 hours after the dropwise addition, filter, and the filtrate is fractionated under normal pressure and collected The fraction at 105-108°C yields N,N-dimethylformamide dimethyl acetal with a yield of 75.3% and a purity of 97%; wherein the molar ratio of sodium methoxide to imine complex is 1:1;

[0038] The ratio of solid sodium methylate and 200# solvent oil in step (2) is that every 1mol sodium methylate is disper...

Embodiment 3

[0040] A kind of synthetic method of N,N-dimethylformamide dimethyl acetal, comprises the following steps:

[0041] (1) Heat N,N-dimethylformamide to 80°C, keep warm, add dimethyl sulfate dropwise, and react for 2 hours after the dropwise addition to obtain an imine complex, cool to room temperature, and set aside; among them, N , the mol ratio of N-dimethylformamide and dimethyl sulfate is 1:1;

[0042] (2) Add solid sodium methoxide to D80 solvent oil, ultrasonically disperse, adjust the temperature to 30°C, keep warm, add the imine complex dropwise, react for 1h after the dropwise addition, filter, and the filtrate is fractionated under normal pressure to collect 105 The fraction at -108°C yields N,N-dimethylformamide dimethyl acetal with a yield of 74.6% and a purity of 97%; wherein the molar ratio of sodium methoxide to imine complex is 1:1;

[0043] The ratio of solid sodium methylate and D80 solvent oil in step (2) is that every 1mol sodium methylate is dispersed in 30...

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Abstract

The invention discloses an N,N-dimethylformamide dimethyl acetal synthesis method. The synthesis method includes: subjecting N,N-dimethylformamide and dimethyl sulfate to reaction to generate an imine complex, and subjecting the imine complex and solid sodium methylate dispersed in an organic solvent to reaction to obtain N,N-dimethylformamide dimethyl acetal, wherein the organic solvent refers to at least one of isoparaffin, solvent oil and white oil. By adoption of the novel organic solvent, reaction conditions (with the temperature being 20-30DEG C) of the imine complex and the sodium methylate can be lowered, and the reaction conditions are milder. In addition, when the reaction temperature is compared with an original reaction temperature ranging from -5 DEG C to 0 DEG C, products generated after reaction are quicker in dissolution and can be timely dissolved in the organic solvent to be wrapped by the organic solvent, so that by-product generation is avoided, and yield is increased. According to experiments, yield of the N,N-dimethylformamide dimethyl acetal can reach 85% above.

Description

technical field [0001] The invention relates to a method for synthesizing a fine pharmaceutical intermediate, in particular to a method for synthesizing N,N-dimethylformamide dimethyl acetal, which belongs to the technical field of fine chemicals. Background technique [0002] N, N-dimethylformamide dimethyl acetal, the English name is N, N-dimethylformamide dimethylacetal, abbreviated as DMF-DMA, the CAS registration number is 4637-24-5, and the molecular formula is C 5 h 13 NO 2 , the molecular weight is 119.16, and the structural formula is: [0003] [0004] N,N-Dimethylformamide dimethyl acetal has a wide range of uses, is an important intermediate in the synthesis of heterocyclic compounds, and is also a good methylation reagent and esterification dehydrating agent, especially as a pharmaceutical synthesis The intermediate can be used in the synthesis of formamidine, 1,2,3-triketones, indole, quinolones, ofloxacin, milrinone and allopurinol and other drugs. [0...

Claims

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Application Information

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IPC IPC(8): C07C213/00C07C217/40
CPCC07C213/00C07C257/06C07C303/24C07C305/04C07C217/40
Inventor 刘玉霞于景民刘菲柴勇利崔炳春李明王大陆张辰高青环
Owner HENAN CHEM IND RES INST
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