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Method for preparing 2,6-dimethyl-2,3-dihydro-1-indanone

A technology of dimethyl and dimethylaniline, applied in the field of chemistry, can solve the problems of complex preparation process, low yield, waste and the like, and achieve the effects of simple preparation steps, good reduction effect, and reduced generation of impurities

Inactive Publication Date: 2019-01-11
ABA CHEM NANTONG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Aiming at the deficiencies of the prior art, the present invention provides a preparation method of 2,6-dimethyl-2,3-dihydro-1-indanone, which has the advantages of higher purity and solves the existing 2, The preparation process of 6-dimethyl-2,3-dihydro-1-indanone is relatively complicated, and the purity of the produced 2,6-dimethyl-2,3-dihydro-1-indanone is not high, so it cannot Completely reacting the reactant causes waste, and the problem that the yield of 2,6-dimethyl-2,3-dihydro-1-indanone is not high during the synthesis process

Method used

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Effect test

Embodiment 1

[0020] A preparation method of 2,6-dimethyl-2,3-dihydro-1-indanone, comprising the following steps:

[0021] 1) In the there-necked flask equipped with mechanical stirring and thermometer, adding concentration is 98% sulfuric acid, then 20 grams of 2,6-dimethylaniline and 30 grams of 2,3-dihydrobenzofuran are added in the three-necked flask, After the dropwise addition, the temperature was raised to 70°C in a water bath, and after stirring for 15 minutes, the temperature was lowered to 50°C. Chlorine gas was continuously introduced and stirred for 20 minutes to obtain 2,6-dimethyl-2,3-dihydrobenzofuran.

[0022] 2) Add the 2,6-dimethyl-2,3-dihydrobenzofuran obtained in step 1) into a two-necked flask equipped with a condensing reflux tube, then add 40 grams of 1-indanone, and add A certain amount of catalyst, use ethanol as a solvent, heat to the reaction temperature, add a certain amount of weak reducing agent, then add a certain amount of hydrazine hydrate, put it in a water...

Embodiment 2

[0027] A preparation method of 2,6-dimethyl-2,3-dihydro-1-indanone, comprising the following steps:

[0028] 1) In the there-necked flask equipped with mechanical stirring and thermometer, adding concentration is 98% sulfuric acid, then 2,6-dimethylaniline 35 grams and 2,3-dihydrobenzofuran 45 grams are added in the there-necked flask, After the dropwise addition, the temperature was raised to 75°C by heating in a water bath, and the temperature was lowered to 55°C after stirring for 17.5 minutes. Chlorine gas was continuously introduced and stirred for 25 minutes to obtain 2,6-dimethyl-2,3-dihydrobenzofuran.

[0029]2) Add the 2,6-dimethyl-2,3-dihydrobenzofuran obtained in step 1) into a two-necked flask equipped with a condensing reflux tube, then add 60 grams of 1-indanone, and add A certain amount of catalyst, use ethanol as a solvent, heat to the reaction temperature, add a certain amount of weak reducing agent, then add a certain amount of hydrazine hydrate, put it in a ...

Embodiment 3

[0034] A preparation method of 2,6-dimethyl-2,3-dihydro-1-indanone, comprising the following steps:

[0035] 1) In the there-necked flask equipped with mechanical stirring and thermometer, adding concentration is 98% sulfuric acid, then 2,6-dimethylaniline 50 grams and 2,3-dihydrobenzofuran 60 grams are added in the there-necked flask, After the dropwise addition, heat up in a water bath to 80°C, stir for 15-20 minutes, then lower the temperature to 60°C, continuously feed chlorine gas, and stir for 30 minutes to obtain 2,6-dimethyl-2,3-dihydrobenzofuran .

[0036] 2) Add the 2,6-dimethyl-2,3-dihydrobenzofuran obtained in step 1) into a two-necked flask equipped with a condensing reflux tube, then add 80 grams of 1-indanone, and add A certain amount of catalyst, use ethanol as a solvent, heat to the reaction temperature, add a certain amount of weak reducing agent, then add a certain amount of hydrazine hydrate, put it in a water bath and heat it for 20 minutes under magnetic...

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Abstract

The invention relates to the technical field of chemistry and discloses a method for preparing 2,6-dimethyl-2,3-dihydro-1-indanone. The method comprises the following steps: 1) adding sulfuric acid having the concentration of 98% into a three-mouth flask filled with a mechanical agitator and a thermometer, adding 20-50g of 2,6-dimethylaniline and 30-60g of 2,3-dihydrobenzofuran into the three-mouth flask, heating in a water bath after dropping completion, raising the temperature to 70-80 DEG C, stirring for 15-20 minutes, reducing the temperature to 50-60 DEG C, continuously introducing chlorine, and stirring for 20-30 minutes, thereby obtaining the 2,6-dimethyl-2,3-dihydrobenzofuran. According to the method for preparing 2,6-dimethyl-2,3-dihydro-1-indanone disclosed by the invention, theoverall preparation steps are simple, and the requirements on hardware facilities of users are low. Moreover, compared with 2,6-dimethyl-2,3-dihydro-1-indanone prepared by the traditional method, the2,6-dimethyl-2,3-dihydro-1-indanone prepared by the method disclosed by the invention has higher purity, and convenience is brought to subsequent application.

Description

technical field [0001] The invention relates to the technical field of chemistry, in particular to a preparation method of 2,6-dimethyl-2,3-dihydro-1-indanone. Background technique [0002] 2,6-Dimethyl-2,3-dihydro-1-indanone is an antioxidant, feed additive or feed additive drug, which can improve the conception rate of dairy cows, the quality of semen of bulls and the fertilization of broiler chickens It can increase the feed remuneration of livestock, poultry and fish and promote growth, improve the conception (sperm) rate of breeding livestock and poultry, improve the quality and vitality of semen, increase milk production, and reduce the occurrence of recessive mastitis and toe hooves. Engage in the oxidation of VE. [0003] The existing 2,6-dimethyl-2,3-dihydro-1-indanone preparation process is relatively complicated, and the produced 2,6-dimethyl-2,3-dihydro-1-indanone The purity is not high, the reactants cannot be reacted completely, resulting in waste, and the yi...

Claims

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Application Information

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IPC IPC(8): C07C45/68C07C49/67
CPCC07C45/68C07D307/79C07C2602/08C07C49/67
Inventor 徐军刘汝章蒋信义
Owner ABA CHEM NANTONG
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