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Synthesis method of p-chloromethyl styrene

A technology of chloromethylstyrene and a synthesis method, which is applied in the fields of dehydrohalogenation preparation, organic chemistry, etc., can solve the problems of high temperature and high pressure, high energy consumption, and high equipment requirements for the reaction, and achieves low pollution, low energy consumption, and reduced energy consumption. side effects

Pending Publication Date: 2019-11-15
山东星顺新材料有限公司
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Problems solved by technology

[0004] The advantage of the above-mentioned gas phase chlorination method is that the single-pass conversion rate of p-methylstyrene is improved, and the product quality is better, but the reaction requires high temperature and high pressure, high equipment requirements, and large energy consumption

Method used

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  • Synthesis method of p-chloromethyl styrene

Examples

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Effect test

Embodiment 1

[0022] Add 23.4g of p-chloromethyl-α-bromoethylbenzene and 92g of toluene into a 500ml four-neck flask, stir to dissolve and clarify, add 6.72g of potassium hydroxide, 2g of 18-crown-6, and react at 40°C for 4 hours. Cool after the reaction, add 100g of water, stir to dissolve, and let stand to separate layers. The upper layer solution was extracted and distilled to obtain 12.5 g of p-chloromethyl styrene with a yield of 81.9%.

Embodiment 2

[0024] Add 23.4g of p-chloromethyl-α-bromoethylbenzene and 92g of toluene into a 500ml four-neck flask, stir to dissolve and clarify, then add 8.4g of potassium hydroxide and 2g of 18-crown-6, and react at 40°C for 4 hours. Cool after the reaction, add 100g of water, stir to dissolve, and let stand to separate layers. The upper layer solution was extracted and distilled to obtain 12.98 g of p-chloromethyl styrene with a yield of 85%.

Embodiment 3

[0026] Add 23.4g p-chloromethyl-α-bromoethylbenzene and 92g toluene into a 500ml four-neck flask, stir to dissolve and clarify, add 11.2g potassium hydroxide, 2g18-crown-6, and react at 40°C for 4 hours. Cool after the reaction, add 100g of water, stir to dissolve, and let stand to separate layers. The upper layer solution was extracted and distilled to obtain 14.5 g of p-chloromethyl styrene with a yield of 95%.

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Abstract

The invention relates to a synthesis method of an organic intermediate, in particular, a synthesis method of p-chloromethyl styrene. According to the synthesis method, a phase-transfer catalytic method is adopted; p-chloromethyl-alpha-bromoethylbenzene and potassium hydroxide are taken as the raw materials; toluene is taken as the solvent; and a phase-transfer catalysis is added to synthesize p-chloromethyl styrene. The synthesis method has the advantages that the reactions are mild, the energy consumption is low, no high pressure or high temperature is needed during the reaction process, thereactants do not react with the solvent or the phase-transfer catalyst, the yield is increased, the side reactions are reduced, and a high quality product is obtained.

Description

technical field [0001] The invention relates to a method for synthesizing an organic intermediate, in particular to a method for synthesizing p-chloromethylstyrene. Background technique [0002] As an organic intermediate, p-chloromethylstyrene has been widely used in various upstream raw materials and downstream products, and is widely used in rubber, ion exchange membranes, adhesives and pesticides. There are various methods for synthesizing p-chloromethylstyrene, including phase transfer catalysis, direct elimination of strong base and high-temperature gas-phase chlorination, etc. And difficult to control and other reasons, many methods can not be applied to actual production. [0003] Chinese patent application CN100560550C adopts the gas-phase chlorination method, takes p-methylstyrene as the reaction raw material, chlorine gas as the halogenation reagent, nitrogen gas as the cycle protection gas, hydroquinone as the polymerization inhibitor, and carbon tetrachloride a...

Claims

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Application Information

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IPC IPC(8): C07C17/25C07C22/04
CPCC07C17/25C07C22/04
Inventor 顾小星
Owner 山东星顺新材料有限公司
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