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Process for preparing P-tertiary butyl phenyl acetic ester organic compounds

A technology for ethyl tert-butyl phenylacetate and organic compounds, which is applied in the field of organic chemical compound preparation, can solve problems such as production and operation hazards, and achieve the effects of simple process and environmental protection

Inactive Publication Date: 2007-04-11
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Because the highly toxic substance cyanide (NaCN) is used in this method, it brings great harm to the production operation

Method used

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  • Process for preparing P-tertiary butyl phenyl acetic ester organic compounds

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] (1), prepare p-tert-butylphenylacetic acid:

[0015] Add 200g p-tert-butylacetophenone and 216g morpholine in a 500ml three-necked flask equipped with a stirrer and a reflux condenser, stir and mix, then add 92g sulfur, and heat the reaction under constant stirring; the temperature gradually rises from 110°C to The reaction temperature is 210°C; it begins to boil at 110°C, and reflux begins at 120°C; the reaction time is 12 hours; then it is cooled to 80°C, and the reaction solution is poured into 500ml of absolute ethanol to obtain yellow precipitated thio-tert-butylmorpholine Amide; put 100g of the yellow precipitate in 150ml of glacial acetic acid and 25ml of 98% sulfuric acid solution for acidification reaction, the reaction temperature is 114-118°C, and the acidification time is 3 hours; then pour the above-mentioned acidified reaction solution into Cool in cold water for 10 hours to obtain the crude product p-tert-butylphenylacetic acid; then recrystallize the cru...

Embodiment 2

[0020] This embodiment is the preparation method of p-tert-butylphenylacetic acid ethyl ester, and its preparation method is exactly the same as above-mentioned embodiment 1 p-tert-butylphenylacetic acid methyl ester.

[0021] (1), prepare p-tert-butylphenylacetic acid: its method is identical with above-mentioned embodiment 1.

[0022] (2), preparation of ethyl p-tert-butylphenylacetate: identical with the method of above-mentioned embodiment 1. The difference is:

[0023] (a) The consumption of raw material is different, adopts p-tert-butylphenylacetic acid 25g, dehydrated alcohol 100ml, sulfuric acid 20ml (98%); (b) when reaction temperature reaches 80 ℃, make it reflux heating 4 hours. The following process steps are exactly the same. Finally, colorless to pale yellow ethyl p-tert-butylphenylacetate was obtained.

[0024] The product has been tested to be 98% pure.

Embodiment 3

[0026] This embodiment is the preparation method of p-tert-butylphenylacetic acid n-butyl ester, and its preparation method is exactly the same as the above-mentioned embodiment 1 p-tert-butylphenylacetic acid methyl ester.

[0027] (1), prepare p-tert-butylphenylacetic acid: its method is identical with above-mentioned embodiment 1.

[0028] (2), preparation of n-butyl p-tert-butylphenylacetic acid: identical with the method of above-mentioned embodiment 1. The difference is: (a) the consumption of raw materials is different, adopt 25g of p-tert-butylphenylacetic acid, 100ml of n-butanol, 20ml of sulfuric acid (98%); . The following process steps are exactly the same. Finally, colorless to pale yellow n-butyl p-tert-butylphenylacetate was obtained.

[0029] The product has been tested to be 98% pure.

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Abstract

The present invention is process of preparing p-tertiary butyl phenylacetic ester compounds and belongs to the field of organic compound preparing technology. The process includes the following steps: 1. thermal reaction of the p-tertiary butyl phenylethyl ketone, morphine and sulfur through stirring in a flask; pouring the reacted liquid into anhydrous alcohol to obtain yellow precipitate; acidifying the precipitate in solution of glacial acetic acid and sulfuric acid and pouring the reacted liquid into cold water to obtain crude p-tertiary butyl phenylacetic acid product; and 2. thermal reaction of the crude p-tertiary butyl phenylacetic acid product, organic alcohol and sulfuric acid into flask at 88-100 deg.c; reflux condensing at 76-80 deg.c; neutralizing with Na2CO3 solution, separate, collecting oil layer and decompression distilling to obtain p-tertiary butyl phenylacetic ester product.

Description

technical field [0001] The invention relates to a preparation method of p-tert-butylphenylacetic acid ester organic compounds (methyl p-tert-butylphenylacetate, ethyl p-tert-butylphenylacetate and n-butyl p-tert-butylphenylacetate), belonging to organic Technical field of chemical compound preparation. Background technique [0002] P-tert-butylphenyl acetate compounds, especially methyl p-tert-butylphenylacetate, is an important synthetic fragrance. The preparation method usually adopted at present is: the raw material p-tert-butyl toluene generates p-tert-butylphenylacetonitrile under the action of NaCN under the action of cyanide, p-tert-butylphenylacetonitrile is hydrolyzed under acidic conditions to obtain tert-butylphenylacetic acid, and then p-tert-butylphenylacetonitrile The esterification reaction of butylphenylacetic acid and alcohol produces p-tert-butylphenylacetic acid ester compounds. Because the highly toxic substance cyanide (NaCN) is used in this method, it...

Claims

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Application Information

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IPC IPC(8): C07C69/612C07C51/305
Inventor 刘秉新徐端钧严惠根
Owner SHANGHAI UNIV
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