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Method for synthesizing n-butyl isocyanate

A technology of n-butyl isocyanate and butyl isocyanate, applied in the field of organic synthesis, can solve the problems of complex process equipment, strong toxicity and long reaction time, and achieve the effects of overcoming complex equipment, mild reaction conditions and short reaction time.

Inactive Publication Date: 2016-03-09
ANHUI GUANGXIN AGROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional synthesis process of n-butyl isocyanate uses n-butylamine, diphenylamine and phosgene as raw materials, and synthesizes products through the phosgene method. This method has many side reactions, low product content, and low yield
The patent (publication number: CN101357898A) of Zheng Jian etc. discloses a kind of method that utilizes reaction tower to improve phosgene method to prepare high-purity n-butyl isocyanate, but this method reaction time is long, and process equipment is complicated, and raw material phosgene is volatile Large, highly toxic, harmful to the environment and human health

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 0.1 mol of n-valeric acid into a 100 ml round bottom flask. The mouth of the bottle is connected with a reflux condenser with a calcium chloride drying tube at the top. Under anhydrous conditions, 0.1 mol of thionyl chloride is added, and the device is placed at 70 After 4 hours of magnetic stirring in the oil bath, the heating is stopped, and the crude product n-valeryl chloride is obtained by distillation under reduced pressure;

[0021] Take the n-valeryl chloride, 40 ml of anhydrous toluene and 0.5 g of phase transfer catalyst tetrabutylammonium bromide obtained in the above steps and put them into a 100 ml three-necked flask. The three-necked flasks are connected to a thermometer. The reflux condenser of the calcium drying tube and a stopper. Put the device in a 60-degree oil bath and stir for 5 minutes. Take 0.1 mol of dry sodium azide and slowly add it to the system under stirring. After reacting until no gas is generated, keep the reaction for 10 minutes, then ...

Embodiment 2

[0023] Add 0.1 mol of n-valeric acid to a 100 ml round bottom flask. The mouth of the bottle is connected to a reflux condenser with a calcium chloride drying tube at the top. Under anhydrous conditions, 0.1 mol of phosphorus trichloride is added, and the device is placed at 70 After 4 hours of magnetic stirring in the oil bath, the heating is stopped, and the crude product n-valeryl chloride is obtained by distillation under reduced pressure;

[0024] Take the n-valeryl chloride, 40 ml of anhydrous toluene and 0.3 g of polyethylene glycol obtained in the above steps and put them into a 100 ml three-necked flask. The three-necked flasks are respectively connected to a thermometer and a reflux with a calcium chloride drying tube on the top. Condenser and a bottle stopper. Put the device in a 60-degree oil bath and stir for 5 minutes. Take 0.1 mol of dry sodium azide and slowly add it to the system under stirring. After reacting until no gas is generated, keep the reaction for 10 m...

Embodiment 3

[0026] Add 0.1 mol of n-valeric acid to a 100 ml round bottom flask. The mouth of the bottle is connected to a reflux condenser with a calcium chloride drying tube at the top. Under anhydrous conditions, 0.1 mol of phosphorus pentachloride is added, and the device is placed at 70 After 4 hours of magnetic stirring in the oil bath, the heating is stopped, and the crude product n-valeryl chloride is obtained by distillation under reduced pressure;

[0027] Take the n-valeryl chloride, 40 ml of anhydrous toluene and 0.7 g of azide trimethylsilane obtained in the above steps and put them into a 100 ml three-necked flask. The three-necked flasks are connected to a thermometer, and one upper mouth is equipped with a calcium chloride drying tube. The reflux condenser and a stopper. Put the device in a 60-degree oil bath and stir for 5 minutes. Take 0.1 mol of dry sodium azide and slowly add it to the system under stirring. After reacting until no gas is generated, keep the reaction for ...

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PUM

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Abstract

The invention discloses a method for synthesizing n-butyl isocyanate. The method comprises the following steps: weighing n-valeric acid and thionyl chloride according to the mole ratio of 1: 1, putting n-valeric acid and thionyl chloride in a round-bottomed flask, enabling an opening of the round-bottomed flask to be connected to a reflux condensing tube, of which an upper opening is provided with a calcium chloride drying tube, carrying out magnetic stirring, heating the round-bottomed flask to the temperature of 60-70 DEG C in oil bath, and carrying out reaction for 4-5 hours, so as to obtain a n-valeryl chloride crude product; and dissolving the crude product and a catalyst in an anhydrous toluene solvent, heating the solution to the temperature of 60-80 DEG C in a three-necked flask, enabling the three-necked flask to be connected to a thermometer, a reflux condensing tube, of which an upper opening is provided with a calcium chloride drying tube, and a flask cork respectively, carrying out magnetic stirring for 5-8 minutes, then, slowly adding drying sodium azide, of which the mole is equal to that of n-valeric acid, carrying out reaction until no gas is produced, keeping the reaction for 10-15 minutes, then, filtering out insolubles, and carrying out rotary evaporation to remove toluene, thereby obtaining n-butyl isocyanate. The method has the advantages of high yield, mild reaction conditions, simplicity in operation, short reaction time and little environmental pollution.

Description

Technical field [0001] The invention relates to the field of organic synthesis, in particular to a method for synthesizing n-butyl isocyanate. Background technique [0002] N-Butyl isocyanate is an important chemical raw material with active chemical properties. It has a wide range of application value in the field of medicine and pesticides. It is mainly used to synthesize IPBC, benomyl and other pesticides, and is also used to develop sulfonylurea herbicides. This type of herbicide has high activity and low toxicity, and has become a key development project at home and abroad. The traditional synthesis process of n-butyl isocyanate uses n-butylamine, diphenylamine and phosgene as raw materials to synthesize the product through the phosgene method. This method has many side reactions, low product content and low yield. The patent (publication number: CN101357898A) applied by Zheng Jian et al. discloses a method for preparing high-purity n-butyl isocyanate by using a reaction to...

Claims

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Application Information

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IPC IPC(8): C07C263/12C07C265/04
CPCC07C263/12C07C265/04
Inventor 过学军胡安胜吴建平高焰兵戴玉婷张军刘长庆徐小兵黄显超朱张
Owner ANHUI GUANGXIN AGROCHEM
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