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New method for simply and conveniently synthesizing chlorocyclohexane

A technology of chlorocyclohexane and cyclohexene, which is applied in the field of synthesizing chlorocyclohexane, can solve the problems of complex catalyst preparation, difficult control, high reaction temperature, etc., and achieve high yield, short reaction time and simple process Effect

Inactive Publication Date: 2011-08-10
PEKING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method has strict requirements on the reactor structure, and the preparation of the catalyst is complicated, the reaction temperature is high, and it is difficult to control.

Method used

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  • New method for simply and conveniently synthesizing chlorocyclohexane
  • New method for simply and conveniently synthesizing chlorocyclohexane
  • New method for simply and conveniently synthesizing chlorocyclohexane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Take by weighing 70g trioctylmethyl ammonium chloride (AT-8) and 30g benzene, after mixing evenly, add the water of 1.5ml, carry out ultrasonic dispersion, make it become reverse phase micelle system, and the water content of control system is in Between 1.5% and 2%.

[0052] Weigh 48g of cyclohexene into the system and mix well.

[0053] Use concentrated sulfuric acid and sodium chloride to react to generate HCl gas, which is continuously fed into the system and kept stirring. The ventilation time is 8h. of the reaction system 1 H NMR spectrum see figure 1 .

[0054] The ventilated mixed solution was placed in a 250ml round-bottomed flask, and was distilled under normal pressure in an oil bath at 100°C to separate benzene (boiling point: 80.1°C) and unreacted cyclohexene (boiling point: 83°C).

[0055] After cooling at room temperature, the atmospheric distillation unit was changed to a vacuum distillation unit, and the temperature of the oil bath was set at 110° ...

Embodiment 2

[0057] Synthetic chlorocyclohexane was prepared in the same manner as in Example 1 except that 65 g of tetramethylammonium chloride was used instead of 70 g of trioctylmethylammonium chloride.

Embodiment 3

[0059] Synthetic cyclohexane chloride was prepared in the same manner as in Example 1 except that 80 g of methyltripropylammonium bromide was used instead of 70 g of trioctylmethylammonium chloride.

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Abstract

The invention relates to a new method for simply and conveniently synthesizing chlorocyclohexane. Hydrochloric acid at superhigh concentration formed in a reverse micelle system can be directly subjected to addition reaction with cyclohexene to form the chlorocyclohexane. In the method, the process is simple, and the chlorocyclohexane with high yield can be obtained at normal temperature in a short time.

Description

technical field [0001] The invention relates to a method for synthesizing chlorocyclohexane by using cyclohexene as a raw material. Background technique [0002] Cyclohexane, also known as cyclohexyl chloride, is a basic raw material for organic synthesis. It plays a very wide role in modern organic synthesis and practical applications. It is mainly used in rubber anti-scorch agent CTP, and can also be used in polyurethane foaming catalysts. Synthesis of N, N-dimethylcyclohexylamine, rust inhibitor, etc., and also an important intermediate for the synthesis of medicines and pesticides. In pesticides, it is used in the synthesis of tricyclohexyl tin chloride, the intermediate of acaricides tricyclotin and triazotin; it can also be used in the synthesis of medicine benzhexol hydrochloride, used in the preparation of antiepileptic and convulsive drugs, etc. [0003] At present, the synthesis methods of chlorocyclohexane mainly include cyclohexanol chlorination method and cyclo...

Claims

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Application Information

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IPC IPC(8): C07C23/10C07C17/08
Inventor 周辉黄昆贺安琪孙燕李晓佩蔡远利徐怡庄吴瑾光
Owner PEKING UNIV
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