CN105566022A - Method for synthesizing oxime ester through transesterification - Google Patents
Method for synthesizing oxime ester through transesterification Download PDFInfo
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Abstract
The invention relates to a method for synthesizing oxime ester through transesterification, and belongs to the technical field of oxime ester synthesis. The method is characterized in that the preparation process comprises: pre-mixing ketoxime and an ester, adding the obtained mixture to a catalytic distillation tower, and carrying out a transesterification reaction under the effect of a sodium methoxide or sodium ethoxide alkaline catalyst to synthesize the oxime ester, wherein a molar ratio of the ketoxime to the ester is 1:(1-2), the amount of the alkaline catalyst is 1-20% of the total mass of the reaction raw material, and the transesterification reaction conditions comprise that the reaction time is 1-8 h, the reaction temperature is 70-130 DEG C, the reaction pressure is 0-2 MPa, rectification is performed on the reaction product, and the solvent is not required during the reaction process. According to the present invention, the catalytic distillation technology is used to carry out the transesterification so as to synthesize the oxime ester, the reaction process is simple, and the conversion rate and the selectivity can achieve more than or equal to 98%.
Description
Technical field
A method for transesterify synthesis oxime ester, belongs to oxime Lipase absobed technical field.
Background technology
Oxime ester is one of the important intermediate of constructing complicated carbon-to-carbon, carbon-heteroatom bond compound.Oxime ester is at synthesis of chiral amine and pharmaceutical intermediate and have in bioactive each heterocyclic compounds and have huge potentiality.Can prepare alkene acid amides easily by oxime ester, further asymmetric catalytic hydrogenation synthesis has optical activity, is widely used in the Chiral Amine compounds of preparation medicine.Chirality pharmacy is the Disciplinary Frontiers of pharmaceutical industries.In recent years, because the high speed development of pharmaceutical industry and chiral drug are in the outstanding representation of clinicing aspect, chiral drug was more and more subject to people's attention, and was also the important directions of future drugs research and development.Chiral Amine compounds produces chiral drug important intermediate.But the amine submerged body that can be used for efficient asymmetric catalytic hydrogenation is at present few, wherein increasingly mature in recent years due to synthetic method of acrylamide compound, is more and more subject to people's attention.But synthesis acrylamide compound important intermediate oxime ester Industrialized synthesis method rarely has report.How to synthesize oxime ester compound is easily current industrial urgent problem.Oxime ester compound belongs to acyl group oxime compound, is a kind of important organic intermediate.Current known method is with ketoxime and acid anhydrides for Material synthesis oxime ester, but transformation efficiency only has 63%, and wastage of material is serious, is not suitable for suitability for industrialized production.
Summary of the invention
The technical problem to be solved in the present invention is: overcome the deficiencies in the prior art, provides the method for a kind of transesterify synthesis oxime ester that a kind of technique is simple, transformation efficiency is high, product purity is high.
The technical solution adopted for the present invention to solve the technical problems is: the method for this transesterify synthesis oxime ester, and it is characterized in that, concrete preparation technology is:
1) will join in the middle part of catalytic distillation tower after reaction raw materials ketoxime and ester premix, under basic catalyst effect, carry out transesterification reaction synthesis oxime ester and obtain by-product alcohol; Ketoxime and ester mol ratio are 1:(1 ~ 2), the amount of basic catalyst is 1% ~ 20% of reaction raw materials total mass, transesterification reaction condition is: the reaction times is 1h ~ 8h, temperature of reaction is 70 DEG C ~ 130 DEG C, reaction pressure is 0 ~ 2MPa, and in ester-exchange reaction, by-product alcohol steams from catalytic distillation column overhead; Described basic catalyst is sodium methylate or sodium ethylate, and reaction raw materials ketoxime is fat hydrocarbon ketoxime, and reaction raw materials ester is fat hydrocarbon ester;
2) reaction product step 1 obtained is carried out rectifying and be get final product, and rectifying condition is: rectifying tower internal pressure is-0.01MPa ~-0.1MPa, and temperature of reaction is 30 DEG C ~ 120 DEG C.
The reaction expression that above-mentioned ketoxime and ester carry out transesterification reaction is:
。
Adopt method provided by the invention, can directly prepare oxime ester from ketoxime.Ketoxime and ester are joined in catalytic distillation tower, under basic catalyst effect, carries out transesterify synthesis oxime ester, the alcohol of generation is distilled away simultaneously.So the temperature in catalytic distillation tower is higher than the boiling point of by-product alcohol, again lower than the boiling point of reaction raw materials ketoxime, preferably close on the boiling point of ketoxime to ensure maximum speed of reaction and productive rate.Coordinate described basic catalyst to carry out transesterification reaction transformation efficiency and selectivity all more than 98%, after rectifying, be separated the product obtained be mainly oxime ester.Reaction process flow process is simple, high financial profit.
The transesterification reaction of ordinary meaning is the permutoid reaction of a kind of ester and alcohol, and the selectivity of this reversible reaction and turnover ratio are general not high.The present inventor successfully obtains oxime ester after replacing alcohol and ester to carry out transesterification reaction with ketoxime, and in this reaction, the control of selectivity and turnover ratio becomes crucial.Although the catalyzer of transesterification reaction is more, but after being applied to the transesterification reaction of ketoxime and ester, the overwhelming majority can not show due catalytic activity, the present invention is using sodium methylate or sodium ethylate as catalyzer, in the absence of a solvent, obviously can increase the selectivity of Exchange Ester Process, ensure the productive rate of oxime ester.
Described reaction raw materials ketoxime is acetoxime, Diacetylmonoxime, 2 pentanone oxime, propione oxime, methyl-n-butyl ketone oxime, 4-methyl-2 pentanone oxime, 2-heptanone oxime, 3-heptanone oxime, dipropyl ketone oxime or valerone.Under condition of the present invention, fat hydrocarbon ketoxime all can reach and reflect effect preferably, but from speed of reaction and the convenient consideration of technology controlling and process, the ketoxime reaction effect of short chain is better.
Preferably, described reaction raw materials ketoxime is acetoxime, Diacetylmonoxime, 2 pentanone oxime or propione oxime.
Described reaction raw materials ester is methyl propionate, butyl propionate, methyl-butyrate, ethyl butyrate, butyl butyrate, isoamyl butyrate, isobutyl isobutyrate, Ethylisovalerate or isoamyl isovalerate.Under condition of the present invention, fat hydrocarbon ester all can reach and reflect effect preferably, but considers from speed of reaction, dealcoholysis rate and raw material sources are convenient, and the ester better effects if of short chain, cost is lower.
Preferably, described reaction raw materials ester is methyl propionate, butyl propionate, methyl-butyrate, ethyl butyrate.
Preferably, first carry out preheating after described reaction raw materials ketoxime and ester premix and join catalytic distillation tower again.Raw material enters catalytic distillation tower after preheat, can reach the temperature needed for reaction, thus reach maximum transformation efficiency within the shorter time within the shorter time.
Preferably, first utilize the waste heat of by-product alcohol to carry out preheating after described reaction raw materials ketoxime and ester premix and join catalytic distillation tower again.Steam from tower top while the by-product alcohol reacted carries out transesterification reaction in catalytic distillation tower, to move to right increase transformation efficiency to impel transesterification reaction, the by-product alcohol steamed has close to the temperature in catalytic distillation tower, by-product alcohol and reaction raw materials is utilized to carry out heat exchange by reaction raw materials preheating, realize the condensation of by-product alcohol simultaneously, by-product alcohol can collect storage after the heat exchange, and reaction raw materials reaches most suitable preheating temperature.Further quickening transesterification reaction efficiency.
In material proportion, the proportioning of ester can promote the transformation efficiency of ketoxime little over amount.The present invention, by adjustment ketoxime and the material ratio of ester and temperature of reaction and reaction pressure, reaches the transformation efficiency of oxime ester and selectivity all more than 98%.Preferably, in the transesterification reaction described in step 1): ketoxime and ester mol ratio are 1:(1.05 ~ 1.2); The amount of basic catalyst is 2% ~ 5% of reaction raw materials total mass; Transesterification reaction condition is: the reaction times is 3h ~ 5h, and temperature of reaction is 72 DEG C ~ 100 DEG C, and reaction pressure is 0 ~ 0.01MPa.
Preferably, step 2) described in rectifying condition be: rectifying pressure is-0.05MPa ~-0.08MPa; Temperature of reaction is 75 DEG C ~ 100 DEG C.
Compared with prior art, the beneficial effect that the method for a kind of transesterify synthesis oxime ester of the present invention has is: the synthetic method of this oxime ester, is for the transesterification reaction of oxime ester prepared by raw material with ketoxime and ester.First ketoxime and ester are used catalytic distillation technology to carry out transesterify under basic catalyst effect and generate oxime ester, then through rectifying, obtain oxime ester sterling, without the need to solvent in reaction process.The present invention adopts catalytic distillation technology to carry out transesterify synthesis oxime ester, and reaction process flow process is simple, and high financial profit, can reduce the production cost of 55%, and transformation efficiency and selectivity all can reach more than 98%.Utilize catalytic distillation tower to realize the distillation of transesterify and by product, utilizing rectifying tower to achieve the refining of product, is a kind of both economical synthetic method, the qualified product purity more than 99% obtained.
Accompanying drawing explanation
Fig. 1 is the preferred a kind of device syndeton schematic diagram of present invention process.
Wherein: 1, raw material pipeline 4 after the first raw material pipeline 2, second raw material pipeline 3, mixing, raw material pipeline 5, by-product alcohol pipeline 6 after heat exchange, by-product alcohol enters storage tank pipeline 7, the thick all-product line 8 of oxime ester, oxime ester qualified product enter storage tank pipeline 9, unreacting material returns mixing tank pipeline 10, mixing tank 11, interchanger 12, catalytic distillation tower 13, product rectifying tower.
Embodiment
With reference to accompanying drawing 1: the preferred a kind of device syndeton schematic diagram of technical process of the present invention, comprise mixing tank 10, interchanger 11, catalytic distillation tower 12, product rectifying tower 13, interchanger 11 is delivered to by raw material pipeline 3 after mixing after the reaction raw materials ketoxime that first raw material pipeline 1 and the second raw material pipeline 2 are sent here by mixing tank 10 and ester mixing, the by-product alcohol returned by by-product alcohol pipeline 5 that reaction raw materials and catalytic distillation tower 12 tower top distill out in interchanger 11 carries out heat exchange, synchronous realization response raw material preheating and the condensation of by-product alcohol, condensation by-product alcohol enters storage tank pipeline 6 by by-product alcohol and sees storage off, reaction raw materials through preheating enters by the middle part of catalytic distillation tower 12, carry out under the effect of basic catalyst transesterification reaction simultaneously by-product alcohol distilled out by tower top.Reaction product is delivered to product rectifying tower 13 through the thick all-product line 7 of oxime ester and is carried out rectifying, oxime ester qualified product are steamed by product rectifying tower 13 tower top, and enter storage tank pipeline 8 by oxime ester qualified product and see storage off, a small amount of excess raw material by the bottom of product rectifying tower 13 tower release, and by unreacting material return mixing tank pipeline 9 be back to mixing tank 10 again mix participate in react.
Below by embodiment, the invention will be further described, but the present invention is not limited only to these examples.Essence of the present invention and invention scope can be fully understood by these embodiments, understand the feature of synthesis of the present invention and separating technology further.Raw material of the present invention is ketoxime and ester, and catalyzer is sodium methylate or sodium ethylate.
Ketoxime is technical grade, purity ﹥ 99%; Ester is technical grade, purity ﹥ 99%; Catalyst sodium methoxide or sodium ethylate are technical grade, purity ﹥ 99%; Described content is mass percent.
Embodiment 1:
3.32kg sodium methylate is dissolved in 73.1kg acetoxime, and with 92.5kg methyl propionate after mixing tank 10 mixes, with catalytic distillation tower 12 tower top material after interchanger 11 heat exchange preheating from continuously feeding in the middle part of catalytic distillation tower 12, transesterification reaction is carried out under controlling bottom temperature 72 DEG C, normal pressure, the methyl alcohol that reaction generates steams from tower top, cools laggard methanol tank through interchanger 11 heat exchange.After reacting 3h in catalytic distillation tower 12, by tower reactor material with being pumped to product rectifying tower 13, under-0.05MPa pressure, under 80 DEG C of conditions, carrying out rectifying, obtaining acetoxime propionic ester 127.7kg, with the acetoxime rate of collecting for 98%, purity is 99.1%.
Embodiment 2:
5.4kg sodium methylate is dissolved in 73.1kg acetoxime, and with 143.2kg butyl propionate after mixing tank mixing, with catalytic distillation tower 12 tower top material after interchanger 11 heat exchange preheating from continuously feeding in the middle part of catalytic distillation tower 12, control bottom temperature 130 DEG C, pressure 0.005MPa carry out transesterification reaction, the butanols that reaction generates steams from tower top, cools laggard butanols tank through interchanger 11 heat exchange.After reacting 4h in catalytic distillation tower 12, by tower reactor material with being pumped to product rectifying tower 13, under-0.06MPa pressure, under 85 DEG C of conditions, carrying out rectifying, obtaining acetoxime propionic ester 127.8kg, with the acetoxime rate of collecting for 98.2%, purity is 99.2%.
Embodiment 3:
5.4kg sodium ethylate is dissolved in 87.12kg Diacetylmonoxime, and with 117.4kg methyl-butyrate after mixing tank mixing, with catalytic distillation tower 12 tower top material after interchanger 11 heat exchange preheating from continuously feeding in the middle part of catalytic distillation tower 12, control bottom temperature 85 DEG C, pressure 0.007MPa carry out transesterification reaction, the methyl alcohol that reaction generates steams from tower top, cools laggard methanol tank through interchanger 11 heat exchange.After reacting 3.5h in catalytic distillation tower 12, by tower reactor material with being pumped to product rectifying tower 13, under-0.07MPa pressure, 90 DEG C are carried out rectifying, obtain Diacetylmonoxime butyric ester 155.6kg, and with the Diacetylmonoxime rate of collecting for 98.4%, purity is 99.5%.
Embodiment 4:
11kg sodium ethylate is dissolved in 87.12kg Diacetylmonoxime, and with 139.4kg ethyl butyrate after mixing tank mixing, through preheating from continuously feeding in the middle part of catalytic distillation tower 12, control bottom temperature 100 DEG C, pressure 0.01MPa carry out transesterification reaction, the ethanol that reaction generates steams from tower top, through the laggard Ethanol tank of condensation.After reaction 5h, by tower reactor material with being pumped to product rectifying tower 13, under-0.08MPa pressure, 92 DEG C are carried out rectifying, obtain Diacetylmonoxime butyric ester 156.2kg, and with the Diacetylmonoxime rate of collecting for 99%, purity is 99.6%.
Embodiment 5:
32.2kg sodium methylate is dissolved in 73.1kg acetoxime, and with 88kg methyl propionate after mixing tank 10 mixes, with catalytic distillation tower 12 tower top material after interchanger 11 heat exchange preheating from continuously feeding in the middle part of catalytic distillation tower 12, transesterification reaction is carried out under controlling tower reactor temperature 70 C, normal pressure, the methyl alcohol that reaction generates steams from tower top, cools laggard methanol tank through interchanger 11 heat exchange.After reacting 8h in catalytic distillation tower 12, by tower reactor material with being pumped to product rectifying tower 13, under-0.01MPa pressure, under 120 DEG C of conditions, carrying out rectifying, obtaining acetoxime propionic ester 127.8kg, with the acetoxime rate of collecting for 98.2%, purity is 99.1%.
Embodiment 6:
3.33kg sodium methylate is dissolved in 73.1kg acetoxime, and with 260kg butyl propionate after mixing tank 10 mixes, with catalytic distillation tower 12 tower top material after interchanger 11 heat exchange preheating from continuously feeding in the middle part of catalytic distillation tower 12, transesterification reaction is carried out under controlling bottom temperature 130 DEG C, 2MPa reaction pressure, the butanols that reaction generates steams from tower top, cools laggard butanols tank through interchanger 11 heat exchange.After reacting 1h in catalytic distillation tower 12, by tower reactor material with being pumped to product rectifying tower 13, under-0.1MPa pressure, under 30 DEG C of conditions, carrying out rectifying, obtaining acetoxime propionic ester 127.6kg, with the acetoxime rate of collecting for 98%, purity is 99.1%.
Comparative example 1
3.32kg sodium hydrate solid is dissolved in 73.1kg acetoxime, and with 92.5kg methyl propionate after mixing tank 10 mixes, with catalytic distillation tower 12 tower top material after interchanger 11 heat exchange preheating from continuously feeding in the middle part of catalytic distillation tower 12, transesterification reaction is carried out under controlling bottom temperature 72 DEG C, normal pressure, the part by product that reaction generates steams from tower top, cools laggard storage tank through interchanger 11 heat exchange.After reacting 3h in catalytic distillation tower 12, by tower reactor material with being pumped to product rectifying tower 13, under-0.05MPa pressure, under 80 DEG C of conditions, carrying out rectifying, obtaining acetoxime propionic ester 69.1kg, with the acetoxime rate of collecting for 53%, purity is 96.1%.Visible when other conditions are all identical with embodiment 1, when using the conventional base catalysis agent sodium hydroxide of transesterification reaction, although can synthesize corresponding oxime ester, the selectivity of reaction is poor, and yield only has 53%.After rectifying, the purity of product is also on the low side.
Comparative example 2
The vitriol oil of 3.32kg mass concentration 98% is dissolved in 73.1kg acetoxime, and with 92.5kg methyl propionate after mixing tank 10 mixes, with catalytic distillation tower 12 tower top material after interchanger 11 heat exchange preheating from continuously feeding in the middle part of catalytic distillation tower 12, transesterification reaction is carried out under controlling bottom temperature 72 DEG C, normal pressure, the part by product that reaction generates steams from tower top, cools laggard storage tank through interchanger 11 heat exchange.After reacting 3h in catalytic distillation tower 12, by tower reactor material with being pumped to product rectifying tower 13, under-0.05MPa pressure, under 80 DEG C of conditions, carrying out rectifying, obtaining acetoxime propionic ester 50.8kg, with the acetoxime rate of collecting for 39%, purity is 96.0%.Visible when other conditions are all identical with embodiment 1, when using the conventional acid vitriol oil of transesterification reaction, the non-constant of selectivity of reaction, yield only has 39%.After rectifying, the purity of product is also on the low side.
Even if comparative example 1 and comparative example 2 are compared with embodiment 1 can find out that, when expecting utilizing transesterify to carry out oxime Lipase absobed, the transformation efficiency of transesterification reaction is low-down under normal conditions, and is not suitable for suitability for industrialized production.
Comparative example 3
3.32kg sodium ethylate is dissolved in 73.1kg acetoxime, and with 92.5kg methyl propionate after mixing tank 10 mixes, with catalytic distillation tower 12 tower top material after interchanger 11 heat exchange preheating from continuously feeding in the middle part of catalytic distillation tower 12, transesterification reaction is carried out under controlling bottom temperature 67 DEG C, normal pressure, the part by product that reaction generates steams from tower top, cools laggard storage tank through interchanger 11 heat exchange.After reacting 3h in catalytic distillation tower 12, by tower reactor material with being pumped to product rectifying tower 13, under-0.05MPa pressure, under 80 DEG C of conditions, carrying out rectifying, obtaining acetoxime propionic ester 97.7kg, with the acetoxime rate of collecting for 75%, purity is 99.0%.Visible when other conditions are all identical with embodiment 1, during the boiling point of transesterification reaction temperature a little more than by-product alcohol, although by-product alcohol can be steamed, due to tower top, to steam thing temperature low, and raw material preheating is not enough; On the other hand because temperature low reaction speed is slow; Under being other condition that embodiment 1 is identical, not exclusively, ultimate yield is lower in reaction.
Comparative example 4
3.32kg sodium ethylate is dissolved in 73.1kg acetoxime, and with 264kg methyl propionate after mixing tank 10 mixes, with catalytic distillation tower 12 tower top material after interchanger 11 heat exchange preheating from continuously feeding in the middle part of catalytic distillation tower 12, transesterification reaction is carried out under controlling bottom temperature 72 DEG C, normal pressure, the part by product that reaction generates steams from tower top, cools laggard storage tank through interchanger 11 heat exchange.After reacting 3h in catalytic distillation tower 12, by tower reactor material with being pumped to product rectifying tower 13, under-0.05MPa pressure, under 80 DEG C of conditions, carrying out rectifying, obtaining acetoxime propionic ester 126.3kg, with the acetoxime rate of collecting for 97%, purity is 97.1%.When the consumption of visible ester in material proportion is too excessive, there will be no raising to the transformation efficiency of reaction, contrary because the amount of isolated by-product alcohol is comparatively large simultaneously, can not remove timely, effecting reaction efficiency can be made to reduce, the yield of final oxime ester decreases.Affect the purity of product after rectifying also on the low side simultaneously.
Comparative example 5
3.32kg sodium hydroxide sodium is dissolved in 73.1kg acetoxime, and with 264kg methyl propionate after mixing tank 10 mixes, with catalytic distillation tower 12 tower top material after interchanger 11 heat exchange preheating from continuously feeding in the middle part of catalytic distillation tower 12, transesterification reaction is carried out under controlling bottom temperature 72 DEG C, normal pressure, the part by product that reaction generates steams from tower top, cools laggard storage tank through interchanger 11 heat exchange.After reacting 3h in catalytic distillation tower 12, by tower reactor material with being pumped to product rectifying tower 13, under-0.05MPa pressure, under 80 DEG C of conditions, carrying out rectifying, obtaining acetoxime propionic ester 73kg, with the acetoxime rate of collecting for 56%, purity is 97.1%.When the consumption of visible ester in material proportion is too excessive, when conventional transesterification catalyst, improving the transformation efficiency of reaction is not clearly, and the yield of oxime ester is lower.
The above is only preferred embodiment of the present invention, and be not restriction the present invention being made to other form, any those skilled in the art may utilize the technology contents of above-mentioned announcement to be changed or be modified as the Equivalent embodiments of equivalent variations.But everyly do not depart from technical solution of the present invention content, any simple modification, equivalent variations and the remodeling done above embodiment according to technical spirit of the present invention, still belong to the protection domain of technical solution of the present invention.
Claims (9)
1. a method for transesterify synthesis oxime ester, it is characterized in that, concrete preparation technology is:
1) will join in the middle part of catalytic distillation tower after reaction raw materials ketoxime and ester premix, under basic catalyst effect, carry out transesterification reaction synthesis oxime ester and obtain by-product alcohol; Ketoxime and ester mol ratio are 1:(1 ~ 2), the amount of basic catalyst is 1% ~ 20% of reaction raw materials total mass, transesterification reaction condition is: the reaction times is 1h ~ 8h, temperature of reaction is 70 DEG C ~ 130 DEG C, reaction pressure is 0 ~ 2MPa, and in ester-exchange reaction, by-product alcohol steams from catalytic distillation column overhead; Described basic catalyst is sodium methylate or sodium ethylate, and reaction raw materials ketoxime is fat hydrocarbon ketoxime, and reaction raw materials ester is fat hydrocarbon ester;
2) reaction product step 1 obtained is carried out rectifying and be get final product, and rectifying condition is: rectifying tower internal pressure is-0.01MPa ~-0.1MPa, and temperature of reaction is 30 DEG C ~ 120 DEG C.
2. the method for transesterify synthesis oxime ester according to claim 1, it is characterized in that: described reaction raw materials ketoxime is acetoxime, Diacetylmonoxime, 2 pentanone oxime, propione oxime, methyl-n-butyl ketone oxime, 4-methyl-2 pentanone oxime, 2-heptanone oxime, 3-heptanone oxime, dipropyl ketone oxime or valerone.
3. the method for transesterify synthesis oxime ester according to claim 1, is characterized in that: described reaction raw materials ketoxime is acetoxime, Diacetylmonoxime, 2 pentanone oxime or propione oxime.
4. the method for transesterify synthesis oxime ester according to claim 1, is characterized in that: described reaction raw materials ester is methyl propionate, butyl propionate, methyl-butyrate, ethyl butyrate, butyl butyrate, isoamyl butyrate, isobutyl isobutyrate, Ethylisovalerate or isoamyl isovalerate.
5. the method for transesterify synthesis oxime ester according to claim 1, is characterized in that: described reaction raw materials ester is methyl propionate, butyl propionate, methyl-butyrate or ethyl butyrate.
6. the method for transesterify according to claim 1 synthesis oxime ester, is characterized in that: first carry out preheating after described reaction raw materials ketoxime and ester premix and join catalytic distillation tower again.
7. the method for transesterify according to claim 1 synthesis oxime ester, is characterized in that: first utilize the waste heat of by-product alcohol to carry out preheating after described reaction raw materials ketoxime and ester premix and join catalytic distillation tower again.
8. the method for transesterify synthesis oxime ester according to claim 1, is characterized in that: in the transesterification reaction described in step 1): ketoxime and ester mol ratio are 1:(1.05 ~ 1.2); The amount of basic catalyst is 2% ~ 5% of reaction raw materials total mass; Transesterification reaction condition is: the reaction times is 3h ~ 5h, and temperature of reaction is 72 DEG C ~ 100 DEG C, and reaction pressure is 0 ~ 0.01MPa.
9. the method for transesterify according to claim 1 synthesis oxime ester, is characterized in that: step 2) described in rectifying condition be: rectifying pressure is-0.05MPa ~-0.08MPa; Temperature of reaction is 75 DEG C ~ 100 DEG C.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08157438A (en) * | 1994-11-30 | 1996-06-18 | Tokuyama Corp | Production of acetyloxime compound |
| CN101337968A (en) * | 2008-08-27 | 2009-01-07 | 湖南大学 | Carboxylic acid rotenonoxime ester, method for preparing same and applications |
| CN102060841A (en) * | 2010-11-26 | 2011-05-18 | 贵州大学 | Acylhydrazone containing heterocyclic amide structure, oxime ester compound and application thereof |
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- 2014-10-08 CN CN201410523387.9A patent/CN105566022B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08157438A (en) * | 1994-11-30 | 1996-06-18 | Tokuyama Corp | Production of acetyloxime compound |
| CN101337968A (en) * | 2008-08-27 | 2009-01-07 | 湖南大学 | Carboxylic acid rotenonoxime ester, method for preparing same and applications |
| CN102060841A (en) * | 2010-11-26 | 2011-05-18 | 贵州大学 | Acylhydrazone containing heterocyclic amide structure, oxime ester compound and application thereof |
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