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Method for synthesizing n-propylbenzene through Grignard reagent method

A technology of Grignard reagent and n-propylbenzene, which is applied in the field of synthesizing n-propylbenzene, can solve the problems of expensive ethyl lithium, harsh reaction conditions, and long reaction time, and achieve low production cost, few side reactions, and simple reaction Effect

Active Publication Date: 2015-09-09
山东东昌精细化工科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It can be seen that the reaction time of this method is longer, and a variety of reagents are used in the reaction, the production cost is higher, and a large amount of aluminum-containing wastewater will be produced, which has a greater impact on the environment
[0009] In addition, n-propylbenzene can also be obtained by reacting benzyl chloride with ethyllithium, but ethyllithium is expensive, its chemical properties are very active, the reaction conditions are harsh, and it must be carried out at an extremely low temperature, which has serious safety hazards. high production cost

Method used

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  • Method for synthesizing n-propylbenzene through Grignard reagent method
  • Method for synthesizing n-propylbenzene through Grignard reagent method
  • Method for synthesizing n-propylbenzene through Grignard reagent method

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Embodiment 1

[0031] Embodiment 1: diethyl ether is made solvent, and benzyl chloride reacts with magnesium powder, then reacts with diethyl sulfate to synthesize n-propylbenzene, and concrete steps are as follows:

[0032] In a 500ml four-necked glass flask with a condensing reflux device, a thermometer, a heating device, a stirring device, and a constant pressure dropping funnel, add 5.2 grams of magnesium powder (0.22mol, an excess of 10%) and 30ml of ether; then add benzyl chloride Mix 26.58 g (0.2 mol) and 70 ml of diethyl ether to form a benzyl chloride solution, add it to a constant pressure dropping funnel, and drop 5 ml of benzyl chloride solution into the flask; add 1 iodine crystal to the flask. Heating initiates the Grignard reaction, and starts stirring to fully mix the materials in the flask. Add the remaining benzyl chloride solution dropwise to the flask, and adjust the rate of addition so that the solvent in the material is in a state of slow reflux.

[0033] After 20 minu...

Embodiment 2

[0035] Example 2: On the basis of Example 1, the solvent was changed to tetrahydrofuran, and the reaction result was (deducting the solvent peak of ether): 8% toluene, 70% n-propylbenzene, and 11% diphenylethane. The boiling point of tetrahydrofuran is high, so that the reaction temperature increases, the selectivity of n-propylbenzene becomes better, and the coupling of benzyl chloride itself is accelerated, and the content of by-product diphenylethane also increases.

Embodiment 3

[0036] Example 3: On the basis of Example 1, the solvent was changed to a mixed solvent of diethyl ether and tetrahydrofuran (each accounting for 50%), and the reaction result was (deducting the diethyl ether solvent peak): 9% toluene, 74% n-propylbenzene, diphenylethyl Alkanes 8%.

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Abstract

The invention relates to a method for synthesizing n-propylbenzene through a Grignard reagent method. The technical scheme comprises that in an ether solvent, benzyl chloride reacts with magnesium powder or magnesium strip to produce a benzyl magnesium chloride Grignard reagent, and the benzyl magnesium chloride Grignard reagent reacts with an ethylation reagent to produce n-propylbenzene. Compared with the method in the prior art, the method for synthesizing the n-propylbenzene by using the Grignard reagent method in the present invention has the following advantages that (1) the reaction is simple, the used reagents are less, and the operation is easy; (2) the pollutants are less, and the method does not produce a lot of aluminum-containing wastewater; (3) the reaction temperature is low and is usually not more than 100 DEG C, the energy consumption is low, and the method does not required the heating evaporation of a large amount of water in the F-C method; and (4) the raw materials are easy to obtain, the yield is high, the side effects are less, and the production cost is low.

Description

technical field [0001] The invention relates to the field of chemical synthesis methods, in particular to a new method for synthesizing n-propylbenzene. technical background [0002] N-propylbenzene (also called n-propylbenzene, propylbenzene) is an aromatic hydrocarbon compound in which one hydrogen atom on the benzene ring is replaced by n-propyl. [0003] N-propylbenzene English name: Propylbenzene or n-Propylbenzene [0004] Molecular Structure: or [0005] Molecular formula: C 9 h 12 , Molecular weight: 120.19, CAS registration number: 103-65-1, density: 0.862, boiling point: 158°C, flash point: 47°C, melting point: -99°C, refractive index: 1.49-1.493. [0006] N-propylbenzene is a colorless liquid at normal temperature and pressure, slightly soluble in water, and soluble in aromatic hydrocarbons, ethanol, ether and other organic solvents. In chemical production, it can be used as solvent or organi...

Claims

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Application Information

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IPC IPC(8): C07C15/02C07C1/32
Inventor 司志华孙海洋焦鹏飞于娜
Owner 山东东昌精细化工科技有限公司
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