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Production method of methyl p-tert-butylphenylacetate

A technology of tert-butylbenzene and methyl acetate, applied in the field of food additive production, can solve the problems of large residues of tert-butyl phenylacetic acid, unreasonable process design, increase of factory cost, etc., so as to shorten the reaction time, improve the product quality, The effect of increasing conversion rates

Pending Publication Date: 2021-12-24
TENGZHOU TIANSHUI BIO TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] 1) The hydrolysis reaction of p-tert-butylphenylacetonitrile is carried out in an acidic environment, and a large amount of acid water, salt and other wastes will be produced during the reaction process, which not only increases the cost of the factory, but also causes environmental pollution
[0009] 2) The existing production process of methyl p-tert-butylphenylacetic acid is unreasonable in process design, the composition of the product is relatively complicated, the residue of p-tert-butylphenylacetic acid is large, the product purity is low, and the aroma of the product is poor

Method used

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  • Production method of methyl p-tert-butylphenylacetate
  • Production method of methyl p-tert-butylphenylacetate
  • Production method of methyl p-tert-butylphenylacetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Method for preparing - methyl tert-butylbenzoacetate: anhydrous methanol and a starting material for t-butyl phytic acid as a starting material, a catalyst for trifluoromethanesulfonic acid, and is prepared by the following reaction operation. Methyl ester:

[0032] 1) Take 1000 ml of three bottles, add anhydrous methanol 300g and 200g of t-butyl phytic acid, catalyst 2G, add, heated reflux reaction, 4 hours, sampling analysis, control to tert-butyl phytic acid ≤ 0.1%, reflow reaction Finish.

[0033] 2) After the reaction is completed, the stream is changed to distillation, and the methanol is recovered at normal pressure to the bottom temperature 80 ° C, and the recovery of 240 g.

[0034] 3) Cooling, standing in layers, removes the lower acid water, the upper organic phase is washed once with 100 g of saturated salt water, and then the organic phase is neutralized with a pure alkaline solution and to pH = 7 ~ 8, then use saturated brine 50 ml × 3 wash To neutral. The cru...

Embodiment 2

[0037] Method for preparation of methyl ester of t-butyl phytate: anhydrous methanol and a starting material for t-butyl phenylacetic acid, trifluoromethanesulfonic acid is a catalyst, and is prepared by the following reaction operation. Phenylacetate:

[0038] 1) Take 1000 ml of three bottles, add 300g of anhydrous methanol and 200g of t-butyl phytic acid, 3G, addition, heating reflow reaction for 4 hours, sampling analysis, control to tert-butyl phytic acid ≤ 0.1%, reflow reaction 5.5 In the end, the reflow reaction ended.

[0039] 2) After the reaction is completed, the stream is changed to distillation, and the methanol is recovered at normal pressure to the bottom temperature 80 ° C, and the recovery of 240 g.

[0040] 3) Cooling, standing in layers, removes the lower acid water, the upper organic phase is washed once with 100 g of saturated salt water, and then the organic phase is neutralized with a pure alkaline solution and to pH = 7 ~ 8, then use saturated brine 50 ml × ...

Embodiment 3

[0043] Method for preparation of methyl ester of t-butyl phytate: anhydrous methanol and a starting material for t-butyl phenylacetic acid, trifluoromethanesulfonic acid is a catalyst, and is prepared by the following reaction operation. Phenylacetate:

[0044] 1) Take 1000 ml of three bottles, add 300g of anhydrous methanol and 200g of t-butyl phytate, 4G, addition, heating reflux for 4 hours, sampling analysis, control to tert-butyl phytic acid ≤ 0.1%, reflow reaction 5.3 In the end, the reflow reaction ended.

[0045] 2) After the reaction is completed, the stream is changed to distillation, and the methanol is recovered at normal pressure to the bottom temperature 80 ° C, and the recovery of 240 g.

[0046] 3) Cooling, standing in layers, removes the lower acid water, the upper organic phase is washed once with 100 g of saturated salt water, and then the organic phase is neutralized with a pure alkaline solution and to pH = 7 ~ 8, then use saturated brine 50 ml × 3 wash To neu...

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Abstract

The invention discloses a production method of methyl p-tert-butylphenylacetate. The method takes p-tert-butylphenylacetic acid and absolute methanol as initial raw materials, and comprises the following reaction operations: heating and refluxing for esterifying and dehydrating p-tert-butylphenylacetic acid and absolute methanol as raw materials under the catalytic action of trifluoromethanesulfonic acid, after the reaction is completed, distilling excessive methanol, cooling residues to room temperature, washing an organic phase once by using a saturated saline solution, standing for layering, separating a water phase, combining the organic phases, neutralizing the organic phases by using 10% sodium carbonate liquid until the pH value is 7-8, standing for layering, separating the water phase, desolventizing the organic phases to the bottom temperature of 80 DEG C, cooling to obtain a crude product, carrying out reduced pressure rectification, and collecting fractions at 122-124 DEG C / 1.2 Kpa to obtain the finished product of the methyl p-tert-butylphenylacetate. The raw materials are easy to obtain and low in price, conditions are easy to control and operate, and the product is low in cost, good in quality and suitable for large-scale production.

Description

Technical field [0001] The present invention relates to the technical field of food additive production, and more particularly to the production method of methyl t-butyl phytate methyl ester. Background technique [0002] Methyl - tert-butylthyl acetate is an aliphatic fragrance. It is a colorless oil liquid, stable in normal temperature, mainly used in modulating chocolate, milky, honey, cream, cheese, tropical fruit, strawberry, vegetables and other flavors. The method of preparing tert-butylbarbide methyl ester is prepared to prepare tert-butylcetones into concentrated sulfuric acid to prepare tert-butylphenylacetic acid, then produce a catalyst, anhydrous methanol as a raw material. This method is high, it is not easy to obtain, difficult to operate, has a large amount of pollution, and a low-cost yield. [0003] Methyl ester, molecular formula is C 13 Hide 18 0 2 , CAS: 3549-23-3 [0004] The structural formula is as follows. [0005] [0006] At present, the synthetic stu...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/614
CPCC07C67/08C07C51/08C07C69/614C07C57/32
Inventor 马兆锋张士金张翔洲李兴华
Owner TENGZHOU TIANSHUI BIO TECH CO LTD
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