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Method for synthetizing alcohol ester acetate by single step of ethyl acetate and alcohol ester exchange

A technology of ethyl acetate and alcohol acetate, applied in the synthesis field of alcohol acetate, can solve the problems such as inability to synthesize alcohol acetate product, increase production cost, inconvenience in popularization and application, and achieves a large market volume and a wide range and saves energy. , beneficial to environmental protection

Inactive Publication Date: 2010-10-06
CHONGQING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] (2) The structure that this method synthesizes ester can only be acetic acid fatty alcohol class material, can not synthesize the acetic acid ester product of higher alcohol more than octyl alcohol, cyclic alcohol, aromatic alcohol, enol etc., and scope of application is limited
[0006] (3) The method adopts a timely extraction process to remove the methanol produced in the exchange process, and reflux methyl acetate enters the reaction system, which requires additional equipment and power, thereby further increasing the production cost
[0007] (4) This method adopts a strong acid catalyst, which has a strong corrosion effect on equipment, large environmental pollution, high cost of decontamination, and is inconvenient for popularization and application

Method used

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  • Method for synthetizing alcohol ester acetate by single step of ethyl acetate and alcohol ester exchange
  • Method for synthetizing alcohol ester acetate by single step of ethyl acetate and alcohol ester exchange
  • Method for synthetizing alcohol ester acetate by single step of ethyl acetate and alcohol ester exchange

Examples

Experimental program
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Effect test

Embodiment 1

[0029] A kind of ethyl acetate and alcohol transesterification one-step method for synthesizing alcohol acetate, its concrete steps are as follows:

[0030] (1) Taking geraniol as a raw material, using cesium carbonate as a catalyst, taking ethyl acetate as an esterification reagent, and also as a solvent, according to geraniol (mmol): cesium carbonate (mmol): ethyl acetate ( Milliliter) ratio is the ratio of 1:0.05:1, in reactor, add cesium carbonate (32.6mg, 0.1mmol) catalyst and ethyl acetate solvent (2.0mL) earlier, under stirring, then add geraniol (308.5mg , 2.0mmol), after the addition was completed, the temperature was raised to 125°C, and the transesterification was carried out with continuous stirring for 25 hours.

[0031] (2) After the (1) step was completed, the alcohol acetate reaction solution prepared in the (1) step was cooled naturally in the air, and the condensing system of the reactor was flushed with dichloromethane, and the washing liquid was incorporate...

Embodiment 2

[0034] A kind of method that ethyl acetate and alcohol transesterification one-step synthetic alcohol acetate, its concrete steps are with embodiment 1, wherein:

[0035] In step (1), take phenylethyl alcohol as raw material, use cesium carbonate as catalyzer, take ethyl acetate as esterification reagent, and do solvent concurrently, according to phenylethyl alcohol (mmol): cesium carbonate (mmol): ethyl acetate (milliliters) ratio is 1:0.01:1 ratio, in reactor, add cesium carbonate (32.6mg, 0.1mmol) and ethyl acetate (10.0mL) first, then add phenethyl alcohol (1.2216g, 10.0mmol) under stirring ), continued to stir and carried out transesterification for 16 hours.

[0036] In step (2), the eluent was a mixture of ethyl acetate:petroleum ether with a volume ratio of 1:80 to obtain phenylethyl acetate (1.5382 g, yield 94%) as a colorless transparent liquid.

Embodiment 3

[0038] A kind of method that ethyl acetate and alcohol transesterification one-step synthetic alcohol acetate, its concrete steps are with embodiment 1, wherein:

[0039] In step (1), take n-octanol as raw material, use cesium carbonate as catalyzer, take ethyl acetate as esterification reagent, and do solvent concurrently, according to n-octanol (mmol): cesium carbonate (mmol): acetic acid The ratio of ethyl ester (milliliter) is the ratio of 1:0.025:0.75, cesium carbonate (162.9mg, 0.5mmol) and ethyl acetate (15.0mL) are added earlier in the reactor, then add n-octanol (2.6046g , 20.0mmol), and continued stirring for 6 hours for transesterification.

[0040] In step (2), n-octyl acetate (3.1006 g, yield 90%) was obtained as a colorless transparent liquid.

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Abstract

The invention discloses a method for synthetizing alcohol ester acetate by a single step of ethyl acetate and alcohol ester exchange, which relates to a synthesis method of the alcohol ester acetate. The method obtains a finished product by taking various alcohol ester acetates as raw materials, carbonate as a catalyst and ethyl acetate as an esterification reagent through single-step ester exchange reaction and concentration and purification. The invention has the characteristics of simple method, simple and convenient operation, energy source saving, low production cost, convenient popularization and application and the like, and diversified alcohol ester products with high yield and good quality can be prepared by adopting the method. The method can be widely applied to the industrial production of the alcohol ester acetate; the products prepared by adopting the method can be widely used as various flavor types of food essences and cosmetic essences, the essences of fancy soaps, washing powders and laundry detergents, the good solvents of dyes and printing ink and the like, and thereby, the demands of high amount due to wide market plane are satisfied.

Description

technical field [0001] The invention belongs to the technical field of organic chemistry synthesis, and in particular relates to a synthesis method of alcohol acetate. Background technique [0002] Alcohol acetate has been widely found as an important structural unit in natural products with biological activity, and many alcohol acetates have high application value, such as benzyl acetate, which has a unique aroma like jasmine, and is used to prepare apples, bananas, etc. , pineapple and other food flavors, and also used as an excellent solvent for alkyd resin, nitrocellulose, dyes, oils, and printing inks. Phenylethyl acetate is used in the preparation of scented soaps and daily cosmetics essences. It can be used as a substitute for methyl heptynoate. It has a peachy aroma and is also commonly used in the preparation of rose, orange blossom, violet, tuberose, briar and other essences. and fruity flavors. Lauryl acetate is a cheap raw material for ester waxy fragrance. It ...

Claims

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Application Information

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IPC IPC(8): C07C67/03C07C69/145C07C69/157C07C69/14C07C69/16C07D307/42C07B41/12
Inventor 熊燕张学强周明凌学戈秦莉晓
Owner CHONGQING UNIV
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