Preparation method of N-alkyl imidazole

A technology for alkyl imidazole and imidazole, applied in the field of synthesizing N-alkyl imidazole, can solve problems such as large energy consumption, and achieve the effect of reducing consumption cost

Inactive Publication Date: 2010-01-27
HUANGGANG NORMAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This leads to high energy consumption in the production process. The current consumption of

Method used

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  • Preparation method of N-alkyl imidazole
  • Preparation method of N-alkyl imidazole

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Embodiment 1

[0019] Embodiment 1: Add 69.3 kilograms (500mol) of 41.84% glyoxal 69.3 kilograms (500mol) and 37.2% formaldehyde 40.3 kilograms (500mol) mixed solution in the reactor 6 of gas-liquid phase synthesis device, open heating steam valve 5 to reactor 6 Carry out heating to 50 ℃, under the situation that stirring blade 7 rotates, open ammonia gas cylinder 12, pass into ammonia gas 21 kilograms (750mol) slowly under micro-negative pressure condition, make liquid-sealed pool 13 almost not have ammonia bubble to emit, according to Measuring scale 11 shows that the data can accurately grasp the amount of ammonia gas charging and discharging, while 55.4 kilograms of methylamine (500mol) aqueous solution of 28% is added dropwise. When the value is fixed, the pump 2 starts to work, and in the absorption tower 17, the ammonia contacts with the sprayed reaction droplets, the ammonia absorption speed is accelerated, and the ammonia pressure drops rapidly. When the ammonia pressure drops below...

Embodiment 2

[0020] Embodiment 2: inject the mixed solution of 69.3 kilograms (500mol) of 41.84% glyoxal and 40.3 kilograms (500mol) of formaldehyde of 37.2% in the reactor of gas-liquid phase synthesis device. Under stirring and controlling slight negative pressure, heat to 50°C, continuously and slowly pass 42 kg (1500mol) of ammonia gas into the mixed aldehyde, and control the temperature at about 55°C. On access to NH 3 During the process, the color of the solution changed from colorless to light yellow, then to golden yellow, orange and finally to brown. Pass through NH 3 After that, it was incubated at 54-55°C for 4h. After the reaction was completed, the water was evaporated, and the fraction at 250°C was collected.

Embodiment 3

[0021] Embodiment 3: Add 69.3 kilograms (500mol) of 41.84% glyoxal and 40.3 kilograms (500mol) of formaldehyde mixed solution of 41.84% in the reactor of gas-liquid phase synthesis device, at 50 ℃, stir and control slight negative pressure Slowly feed 21 kilograms (750mol) of ammonia gas, and simultaneously add 76 kilograms (500mol) of 30% ethylamine solution dropwise; after the addition, continue to control the temperature at 50°C and react for 6 hours; The water was removed and the fraction at 150°C was collected.

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Abstract

The invention relates to a preparation method of N-alkyl imidazole, solves the problems of high moisture evaporation capacity and high energy consumption of the prior art and is characterized in that alkyl residue, ammonia, formaldehyde and glyoxal are taken as raw materials to synthetize the N-alkyl imidazole. Namely mixed solution of glyoxal and formaldehyde is added into a kettle; ammonia is led in under the condition that temperature and pressure are controlled while alkylamine solution is dropwise added; after charging, the temperature and pressure are continuously controlled and reaction is carried out for six hours; after the reaction is completed, water is boiled off under the condition that pressure is reduced (4000Pa), and fraction at certain temperature is collected. The invention adopts ammonia instead of ammonia water or ammoniacal brine solution in reaction, so that water to be boiled off is reduced and production cost of alkyl imidazole is greatly reduced.

Description

1. Technical field [0001] The invention relates to a method for synthesizing N-alkylimidazoles, in particular to a method for synthesizing N-alkylimidazoles by using alkylammonia, ammonia gas, formaldehyde and glyoxal as raw materials. 2. Background technology [0002] The structural formula of N-alkylimidazole is: [0003] [0004] Where: R=H or -CH 3 or -CH 2 CH 3 . [0005] N-alkylimidazoles are often used as drugs, antibacterial agents, enzyme inhibitors and other fine chemicals, and are important raw materials or intermediates in chemical or pharmaceutical industries (such as synthesizing antifungal, treating microcirculation disorders, inflammation and inhibiting tumor metastasis, etc.) . The methods for the synthesis of N-alkylimidazoles that have been reported so far are: alkylammonia (水溶液) + ammonia (水) + formaldehyde (水溶液) +Glyoxal (水 溶液) →N-Alkylimidazole; Alkylamine (水溶液) + formaldehyde (水溶液) +Glyoxal (水溶液) + ammonia (水) →N-Alkylimidazole; Alkyla...

Claims

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Application Information

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IPC IPC(8): C07D233/58
Inventor 曾舟华刘焕彬熊绪杰徐振强曾昆
Owner HUANGGANG NORMAL UNIV
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