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Method for preparing 2-methyl-3-phenyl benzil alcohol

A technology of phenyl benzyl alcohol and methyl biphenyl is applied in the field of preparation of 2-methyl-3-phenyl benzyl alcohol, can solve the problems of low activity, low process yield, low product content and the like, and achieves the yield High performance, good product purity and convenient process operation

Inactive Publication Date: 2007-03-28
荆和祥
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The preparation method of existing 2-methyl-3-phenylbenzyl alcohol has: take 2,6-dichlorotoluene as raw material through two-step format reaction, prepare product with the direct reaction of formaldehyde gas, because chlorine atom and formaldehyde in the raw material The activity of the reaction is low, the yield of this process is low, and the content of the obtained product is not high

Method used

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  • Method for preparing 2-methyl-3-phenyl benzil alcohol

Examples

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specific example 1

[0035] Add 130g of magnesium chips into a 2000ml four-necked bottle, then add 1000g of tetrahydrofuran and stir, add 0.65g of iodine to initiate the reaction, then raise the temperature to reflux and add 750g of 2,6-dichlorotoluene dropwise, the dropping temperature is kept at reflux, and the dropwise addition is completed Afterwards, reflux and keep warm for 1 hour, and set aside.

[0036] Add 750g of bromobenzene, 50g of tetrahydrofuran and 2g of activated carbon loaded with a metal nickel halide compound into a 2000ml four-necked flask, raise the temperature to reflux, add the above reaction solution dropwise, and reflux for 2 hours after the dripping is completed. The above reaction solution was poured into 5% dilute sulfuric acid solution for hydrolysis, and the hydrolysis temperature was controlled at 30°C. Heating up to the kettle temperature of 100°C for precipitation, stopping, cooling down to normal temperature, and stratifying. After the lower water layer was separ...

specific example 2

[0040] Add 260g of magnesium chips into a 5000ml four-necked bottle, then add 2200g of tetrahydrofuran and stir. After adding 1.5g of iodine to trigger, the temperature is raised to reflux and 1400g of 2,6-dichlorotoluene is added dropwise. The dropping temperature is kept at reflux. After the dropwise addition is completed Reflux for 1 hour and set aside.

[0041] Add 1400g of benzene bromide, 110g of tetrahydrofuran and 3.5g of activated carbon loaded with a metal nickel halide compound into a 5000ml four-neck flask, raise the temperature to reflux, add the above reaction solution dropwise, and reflux for 2 hours after the dripping is completed. The above reaction solution was poured into 5% dilute sulfuric acid solution for hydrolysis, and the hydrolysis temperature was controlled at 30°C. Heating up to the kettle temperature of 100°C for precipitation, stopping, cooling down to normal temperature, and stratifying. After the lower water layer was separated, the oil layer w...

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Abstract

The invention belongs to the technical field of chemical product preparing method, especially a 2-methyl-3-phenyl benzylalcohol preparing method, comprising the main steps of: 1) using 2, 6-dichlorotoluene to make one-step formatting reaction in tetrahydrofuran solvent and then reacting with benzene bromide under the action of catalyst to produce an intermediate 3-chloro-2-methylbiphenyl; 2) making the intermediate perform two-step formatting reaction in tetrahydrofuran solvent and then directly reacting with dimethylformamide to produce 2-methyl-3-phenyl benzaldehyde; 3) reducing 2-methyl-3-phenyl benzaldehyde with metal reducer to produce course 2-mehtyl-3-phenyl benylalcohol; and 4) refining the course product with methanol, alcohol, toluene, activated carbon, etc and obtaining the finished product. And it is convenient to operating, beneficial to large-scale industrialized production, produces fewer three wastes and has advantages of high product yield and good product purity.

Description

technical field [0001] The invention belongs to the technical field of preparation methods of chemical products, in particular to a preparation method of 2-methyl-3-phenylbenzyl alcohol. Background technique [0002] The molecular formula of 2-methyl-3-phenylbenzyl alcohol is C 14 h 14 O, the molecular weight is 198, and the structural formula is: [0003] [0004] 2-Methyl-3-phenylbenzyl alcohol is a white crystal with a special smell of alcohol. Soluble in toluene, methanol, ethyl acetate, acetone and other organic solvents, insoluble in water. This product is mainly used in the production of the pesticide bifenthrin and the synthesis of other pharmaceutical products. [0005] The preparation method of existing 2-methyl-3-phenylbenzyl alcohol has: take 2,6-dichlorotoluene as raw material through two-step format reaction, prepare product with the direct reaction of formaldehyde gas, because chlorine atom and formaldehyde in the raw material The activity of the react...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C33/24C07C29/14C07C29/36
CPCY02P20/52
Inventor 荆和祥王海峻
Owner 荆和祥
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