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A kind of preparation method of 2-methyl-3-phenylbenzyl alcohol

A technology of phenylbenzyl alcohol and dimethylbiphenyl, which is applied in the field of preparation of 2-methyl-3-phenylbenzyl alcohol, can solve the problems of cumbersome operation, high cost, and high equipment requirements, and achieve simple operation and low The effect of raw material cost and reduction of equipment requirements

Active Publication Date: 2016-01-20
JIANGSU LIANHE CHEM TECH +4
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The technical problem to be solved by the present invention is that, in order to overcome the defects of the prior art that the preparation method of 2-methyl-3-phenylbenzyl alcohol has high cost, cumbersome operation, high requirements on equipment, and is unfavorable for industrialized production, and A preparation method of 2-methyl-3-phenylbenzyl alcohol is provided

Method used

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  • A kind of preparation method of 2-methyl-3-phenylbenzyl alcohol
  • A kind of preparation method of 2-methyl-3-phenylbenzyl alcohol
  • A kind of preparation method of 2-methyl-3-phenylbenzyl alcohol

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Effect test

Embodiment 1

[0057] Add 182.3g of 2,3-dimethylbiphenyl (DMBP) into a 500mL four-neck bottle, heat up to 80 degrees, turn on the light, and start to introduce chlorine gas. The temperature is controlled within 100 degrees, and the conversion rate is about 70% when the gas phase is detected. Finally, stop the chlorine flow and blow nitrogen into it to take away the remaining chlorine and hydrogen chloride. The reaction solution was distilled under reduced pressure. The first fraction was 51.9 g, which was unreacted 2,3-dimethylbiphenyl, and the yield was 28.5%. The middle distillate is 2-chloromethyl-3-methylbiphenyl (CMMBP), 82.6g, yield 38.1%, which can be used for the reaction of preparing 2,3-dimethylbiphenyl. The final fraction is mainly 2-methyl-3-chloromethylbiphenyl (MCMBP), 62.8g, with a yield of 29.0%, which can be used for the subsequent preparation of 2-methyl-3-phenylbenzyl alcohol.

Embodiment 2

[0059] Add 182.3g of 2,3-dimethylbiphenyl (DMBP) and 4.2g of phosphorus pentachloride into the four-necked bottle, after the temperature rises to 80°C, turn on the light, start to feed chlorine gas, control the temperature below 100°C, and wait for gas phase detection After the conversion rate is about 70%, slowly add 42.0g of 20% NaHCO dropwise under ice bath 3 solution. The extraction was separated and the organic phase was distilled under reduced pressure. The first fraction was 53.8g, which was unreacted 2,3-dimethylbiphenyl, and the yield was 29.5%. The middle distillate is 2-chloromethyl-3-methylbiphenyl (CMMBP), 84.3g, yield 38.9%, used for the reaction of preparing 2,3-dimethylbiphenyl. The final fraction is mainly 2-methyl-3-chloromethylbiphenyl (MCMBP), 64.1g, with a yield of 29.6%, which can be used for the subsequent preparation of 2-methyl-3-phenylbenzyl alcohol.

Embodiment 3

[0061] Add 182.3g of 2,3-dimethylbiphenyl (DMBP) and 4.2g of phosphorus pentachloride into the four-necked bottle, and after the temperature rises to 40°C, turn on the light, and start to introduce chlorine gas, and wait until the conversion rate is about 70% by gas phase detection , Slowly add 42.0g of 20% NaHCO3 solution dropwise under ice bath. The extraction was separated and the organic phase was distilled under reduced pressure. The first fraction was 56.5 g, which was unreacted 2,3-dimethylbiphenyl, and the yield was 31.0%. The middle distillate is 2-chloromethyl-3-methylbiphenyl (CMMBP), 80.2g, yield 37.0%, used for the reaction of preparing 2,3-dimethylbiphenyl. The final fraction is mainly 2-methyl-3-chloromethylbiphenyl (MCMBP), 57.2g, yield 26.4%, which can be used for subsequent preparation of 2-methyl-3-phenylbenzyl alcohol.

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Abstract

The invention relates to a preparation method of 2-methyl-3-phenyl benzyl alcohol. The preparation method comprises the steps of (1) under a lighting condition, enabling 2,3-dimethyl biphenyl to mix and react with chlorine gas at 40-120 DEGC; or, in the presence of an initiator, enabling the 2,3-dimethyl biphenyl to react with sulfuryl chloride or chlorine gas at 40-120 DEG C; (2) implementing an esterification reaction on 2-methyl-3-chloromethyl biphenyl prepared by the step (1) and an esterification reagent in a solvent in the presence of a catalyst; and (3) under an alkaline condition, hydrolyzing an esterification product prepared by the step (2), and controlling pH range within 9-14. The preparation method disclosed by the invention is simple and convenient to operate, relatively low in cost, not high in requirement on equipment and applicable to industrial production. (img file='DDA0000466672690000011. TIF'wi='1528'he='344' / ).

Description

technical field [0001] The invention relates to a preparation method of 2-methyl-3-phenylbenzyl alcohol. Background technique [0002] 2-Methyl-3-phenylbenzyl alcohol is an important intermediate in the production of the pesticide bifenthrin and other pesticides. [0003] There are four main methods for preparing 2-methyl-3-phenylbenzyl alcohol at present: [0004] The first method is to use 2,6-dichlorotoluene as a raw material, THF as a solvent, react with bromobenzene under a catalyst after one-step Grignard reaction to obtain 3-chloro-2-methylbiphenyl, and then carry out in THF In the second step, the Grignard reaction directly reacts with formaldehyde gas or paraformaldehyde to obtain the target product. [0005] The second method (CN1935761A, CN101130485A) uses 2,6-dichlorotoluene as a raw material, THF as a solvent, and reacts with bromobenzene under a catalyst to prepare 3-chloro-2-methylbiphenyl after a one-step reaction. Then carry out the second-step Grignard r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C33/24C07C27/02
CPCC07C17/14C07C29/095C07C67/11C07C33/24C07C22/04C07C69/157
Inventor 樊小彬林行军周述勇陈冬辉徐晓明黄超沈启富
Owner JIANGSU LIANHE CHEM TECH