Synthesizing method for 1,3, dimethyl-2-imidazolidinone

A technology of imidazolinone and synthesis method, applied in 1 field, can solve problems such as inability to use, and achieve the effects of improving utilization rate, easy control of reaction conditions, and reducing material cost

Inactive Publication Date: 2007-11-14
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This synthetic method needs to use 85% mass percentage concentration formic acid as reaction medium, and can't use to lower than 85% mass percentage concentration formic acid

Method used

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  • Synthesizing method for 1,3, dimethyl-2-imidazolidinone
  • Synthesizing method for 1,3, dimethyl-2-imidazolidinone
  • Synthesizing method for 1,3, dimethyl-2-imidazolidinone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Add 501g (3.626mol) 33.3% formic acid, 107g paraformaldehyde (3.567mol based on formaldehyde) and 153g (1.779mol) 2-imidazoline to a 1000mL four-day bottle equipped with stirring, thermometer, and reflux condenser Ketone, stirred, heated to 70°C, reacted for 4 hours, then added 237g (4.379mol) 85% formic acid, heated and refluxed for 12 hours, and distilled out the formic acid. The reactant was neutralized with sodium hydroxide solution, vacuum distilled, and the 105°C-118°C fraction was collected at a vacuum degree of 0.095Mpa to obtain 1,3-dimethyl-2-imidazolidinone with a purity of 99.7% by gas chromatography. Yield 78%.

[0030] bp=225.5°C

[0031] IR (KBr cm -1 ) 1249 1290, 1504, 1699, 2862, 2938

example 2

[0033] In a 1000mL four-necked flask equipped with stirring, a thermometer, and a reflux condenser, add 475g (4.234mol) of 41.8% formic acid, 117g of paraformaldehyde (calculated as 3.900mol by formaldehyde), 153g (1.779mol) of 2-imidazoline Ketone, stirred, heated to 80°C, reacted for 3 hours, then added 195g (3.985mol) 94% formic acid, heated to reflux for 12 hours, evaporated 413g of formic acid, the concentration of formic acid was 45%. The reactant was neutralized with sodium hydroxide solution, vacuum distilled, and the 105°C-118°C fraction was collected at a vacuum degree of 0.095Mpa to obtain 1,3-dimethyl-2-imidazolidinone with a purity of 99.9% by gas chromatography. Yield 79.2%.

[0034] bp=225.5°C

[0035] IR (KBr cm -1 ) 1249 1290, 1504, 1699, 2862, 2938

example 3

[0037] In the 1000mL four-neck flask equipped with stirring, thermometer, and reflux condenser, add 170g paraformaldehyde (calculated as 5.667mol by formaldehyde), the formic acid 413g (4.040mol) of example 2 reclaims 45% formic acid, 153g (1.779mol ) 2-imidazolinone, stirred, heated to 90°C, reacted for 2 hours, then added 216g (3.985mol) 85% formic acid, heated to reflux for 12 hours, distilled 467g of dilute formic acid, the concentration was 41%. The reactant was neutralized by adding sodium hydroxide solution, vacuum distilled, and the 105°C-118°C fraction was collected at a vacuum degree of 0.095Mpa to obtain 1,3-dimethyl-2-imidazolidinone, whose purity by gas chromatography analysis was 99.93%. Yield 81.3%.

[0038] bp=225.5°C

[0039] IR (KBr cm -1 ) 1249 1290, 1504, 1699, 2862, 2938.

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Abstract

This invention relates to synthetic method of 1, 3 - dimethyl - 2-imidazolidinone. The invention solves the problem in exsiting method that the reaction need 85% concentration methanoic acid as reaction medium, and the generated methanoic acid has no means of reusing. The invention takes paraformaldehyde and 2-imidazolidinone as raw material, 30% to 45%methanoic acid as reaction medium. Firstly proceed paraformaldehyde depolymerization, then add 85%or 94% methanoic acid, warm-up till circumfluence reaction for 12 hours, then gain 1, 3 - dimethyl - 2-imidazolidinone. The invention could cyclic utilize sparse methanoic acid generated from 1, 3 - dimethyl - 2-imidazolidinone synthetic reaction, thereby advance capacity utilization rate, depress manufacturing cost.

Description

technical field [0001] The invention relates to a synthesis method of 1,3-dimethyl-2-imidazolinone, which belongs to organic synthesis and is mainly used for the preparation of 1,3-dimethyl-2-imidazolidinone. Background technique [0002] 1,3-Dimethyl-2-imidazolinone (hereinafter referred to as DMI) is a colorless and transparent liquid with high boiling point, low toxicity, low melting point, acid and alkali resistance, hydrolysis resistance, and light-oxygen stability. Polar inert solvent. DMI has excellent solubility to inorganic substances, organic substances and various resins, and is an important organic solvent widely used in organic synthesis. [0003] DMI synthesis methods are: (a) carbon dioxide method; (b) phosgene method; (c) urea method; (d) imidazolinone method. The carbon dioxide method requires high-temperature and high-pressure equipment, the equipment investment is too large, and the process requirements are strict; the phosgene method is highly toxic, an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D233/34
Inventor 姬明理杨毅马玲姚转乐岁文豪刘建韬刘鸿
Owner XIAN MODERN CHEM RES INST
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