CN109678699A - A kind of milk lactone spice is continuously synthesizing to method - Google Patents
A kind of milk lactone spice is continuously synthesizing to method Download PDFInfo
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- CN109678699A CN109678699A CN201910086917.0A CN201910086917A CN109678699A CN 109678699 A CN109678699 A CN 109678699A CN 201910086917 A CN201910086917 A CN 201910086917A CN 109678699 A CN109678699 A CN 109678699A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/45—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by condensation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/09—Preparation of carboxylic acids or their salts, halides or anhydrides from carboxylic acid esters or lactones
Abstract
The invention belongs to synthetic perfume technical fields, it is continuously synthesizing to method more particularly to a kind of milk lactone spice, is included under buck action condition and carries out aldol reaction, then hydrogenated reaction, Baeyer-Villiger oxidation, through sour continuous hydrolyzing, dehydration obtains milk lactone spice；The aldol reaction includes: that the cyclohexanone by part as bottom material is uniformly mixed with buck, heat treatment, the mixture of surplus cyclohexanone and n-butanal is added dropwise, stir when being added dropwise, and continue after completion of dropwise addition to stir, reaction was completed below 1% for the content of insulation reaction to n-butanal；Oil reservoir is separated after standing, collects water layer and recovery；It collects oil reservoir and is transferred to after washing process in distillation still and be distilled to recover excessive cyclohexanone and apply, collect the condensation product of bottom；The present invention improves the yield of the aldol reaction by the way that cyclohexanone to be added in different ways；Also, under the conditions of reaction temperature of the invention, can a step obtain the product of aldol condensation.
Description
Technical field
The invention belongs to synthetic perfume technical fields, and in particular to a kind of milk lactone spice is continuously synthesizing to method.
Background technique
Milk lactone is 5 or 6- decene acid blend, CAS 72881-27-7, English name: Milk lactone, 5 (6)-
Decenoic acids mixture is a kind of fragrance product with milk fragrant smell.It is actually a kind of unsaturated fat
Acid, this minimal amount of unsaturated fatty acid can produce milk fragrance, give off a strong fragrance, and lasting fragrance is U.S. utility fragrance system
The safe edible fragrance of NAB National Association 0f Broadcasters' approval is made, application range is extremely extensive, is the food such as milk, cream, cheese essence, chocolate
The important source material of product.It in addition, milk lactone boiling point is high, can be used in bakery, be easy quilt unlike compounding milk flavour
It destroys, application prospect is very wide.
Chinese patent CN1266841A uses n-butanal and cyclohexanone for raw material, through alkaline condensation, selective hydrogenation, peroxide
Change hydrogen ring expansion is lactone, and finally dehydration obtains 5 (6)-decylenic acid in acid condition, and in alkaline condensation, reaction is slow for the reaction,
And reaction yield is low, separating-purifying processing is cumbersome, and leading to entire synthetic route, there is at high cost, severe reaction conditions, operation
The disadvantages of complexity, low yield.
Chinese patent CN103864601A uses n-butanal, cyclohexanone for starting material, by making in phase transfer catalyst
Aldol alkaline condensation reaction under, aoxidizes through catalytic hydrogenation, Baeyer-Villiger after, is most dehydrated afterwards through sour water solution
To 5 (6)-decylenic acid.The reaction is utilizing at room temperature using phase reforming catalyst condensation, subsequent to need that solvent dehydration is added,
The disadvantages of leading to entire synthetic route there is at high cost, severe reaction conditions, complicated for operation, low yield.In subsequent decarboxylation
In the process, which reacts under strongly acidic conditions, can generate a large amount of strong acid waste water and generate.
Summary of the invention
It is an object of the invention to overcome deficiency in the prior art, a kind of high yield is provided, inexpensive and operation is more
Simple milk lactone spice is continuously synthesizing to method.
To achieve the goals above, the present invention is achieved by the following scheme:
A kind of milk lactone spice is continuously synthesizing to method, and the synthetic method includes being with n-butanal and cyclohexanone
Raw material carries out aldol reaction under buck action condition, then hydrogenated reaction, Baeyer-Villiger oxidation, finally
Through sour continuous hydrolyzing, dehydration obtains the milk lactone spice；
The specific steps of the aldol reaction include: that the cyclohexanone by part as bottom material is uniformly mixed with buck,
The mixture of surplus cyclohexanone and n-butanal is then added dropwise in heat treatment, stirs when being added dropwise, and continue after completion of dropwise addition
Stirring, reaction was completed below 1% for insulation reaction to the content for detecting n-butanal；
Oil reservoir is separated after standing, collects water layer and recovery；Oil reservoir is collected to be transferred in distillation still after washing process
It is distilled to recover excessive cyclohexanone to apply, collects the condensation product of bottom.
Preferably, in the step of aldol reaction, the mass fraction of the buck is 0.5%~5.0%.
Preferably, in the step of aldol reaction, control heating temperature is 50~100 DEG C, controls surplus ring
The time for adding of the mixture of hexanone and n-butanal is 2~8h.
Preferably, the specific steps of the hydrogenation reaction include: that the condensation for the bottom that will be obtained after aldol reaction produces
Object is added in high-pressure hydrogenation reaction kettle, and hydrogenation reaction solvent is added and Pd/C catalyst, room temperature add hydrogen until not inhaling hydrogen, steams
Evaporate recycling hydrogenation reaction solvent apply after, obtain intermediate product 2- butyl cyclohexanone.
Preferably, the hydrogenation reaction solvent is selected from one of petroleum ether, hexamethylene, dichloroethanes.
Preferably, the specific steps of the Baeyer-Villiger oxidation include: that acetic acid is uniformly mixed system with hydrogen peroxide
It is standby at spare after Peracetic acid, Peracetic acid is slowly dropped in intermediate product 2- butyl cyclohexanone, stirring to reaction terminates；
Water is added into the product after reaction, stirring is washed to neutrality, ε-decalactone is obtained after stratification.
Preferably, the temperature control of the Baeyer-Villiger oxidation reaction is at 5~30 DEG C, and the reaction time is 2~
12h。
Preferably, the specific steps of the continuous hydrolyzing include: dropwise addition ε-decalactone in oxytropism solution, when being added dropwise
Stirring terminates to reaction, and stratification, oil reservoir is washed to neutrality, obtains milk lactone spice crude product；By milk lactone spice
Crude product is evaporated under reduced pressure to obtain final product milk lactone spice.
Preferably, the acid solution is selected from one of sulfuric acid, phosphoric acid, hydrochloric acid；The quality of the acid solution point
Number is 1.0%~50%.
Preferably, the condition of the vacuum distillation include: control vacuum pressure be 667~3333Pa, temperature be 135~
160℃。
Compared with prior art, the present invention has following technical effect that
In technical solution provided by the invention, carry out aldol reaction under alkaline condition, by by cyclohexanone with not
Same mode is added in reaction system, improves the yield of the aldol reaction；Also, in reaction temperature item of the invention
Under part, can a step obtain the product of aldol condensation；
In the present invention, stratification is carried out by the reaction product to aldol reaction, the buck of water layer is returned
Receipts are applied, and not only will not influence the yield of reaction, moreover it is possible to the effective generation for reducing waste water, and improve the utilization rate to buck；
In technical solution provided by the invention, successive reaction is utilized during sour continuous hydrolyzing, reduces acidity
The use total amount of solution, realizes and is continuously synthesizing to milk lactone spice, increases the output of product.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment.
Specific embodiment
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below
Specific embodiment is closed, the present invention is furture elucidated.
All raw materials in the present invention, are not particularly limited its source, buying on the market or according to this field skill
The preparation of conventional method known to art personnel.
All raw materials in the present invention, are not particularly limited its purity, and present invention preferably employs analyze pure or composite wood
The conventional purity that material field uses.
The present invention provides a kind of method that is continuously synthesizing to of milk lactone spice, the synthetic method includes with positive fourth
Aldehyde and cyclohexanone are raw material, aldol reaction are carried out under buck action condition, then hydrogenated reaction, Baeyer-
Villiger oxidation, most afterwards through sour continuous hydrolyzing, dehydration obtains the milk lactone spice；
The specific steps of the aldol reaction include: that the cyclohexanone by part as bottom material is uniformly mixed with buck,
The mixture of surplus cyclohexanone and n-butanal is then added dropwise in heat treatment, stirs when being added dropwise, and continue after completion of dropwise addition
Stirring, reaction was completed below 1% for insulation reaction to the content for detecting n-butanal；
Oil reservoir is separated after standing, collects water layer and recovery；Oil reservoir is collected to be transferred in distillation still after washing process
It is distilled to recover excessive cyclohexanone to apply, collects the condensation product of bottom.
In technical solution provided by the invention, carry out aldol reaction under alkaline condition, by by cyclohexanone with not
Same mode is added in reaction system, improves the yield of the aldol reaction；Also, in reaction temperature item of the invention
Under part, can a step obtain the product of aldol condensation；In the present invention, stood by the reaction product to aldol reaction
Layering carries out recovery to the buck of water layer, not only will not influence the yield of reaction, moreover it is possible to the effective production for reducing waste water
It is raw, and improve the utilization rate to buck；In technical solution provided by the invention, using continuous during sour continuous hydrolyzing
Reaction, reduces the use total amount of acid solution, realizes and be continuously synthesizing to milk lactone spice, increase the output of product.
Further, according to the present invention, the ratio of the n-butanal and cyclohexanone, and as bottom material cyclohexanone and with
The ratio of the cyclohexanone of the surplus of n-butanal mixing can select in a wider scope, in order to ensure higher reaction effect
Rate, the present invention in, the additive amount of the n-butanal and total cyclohexanone is calculated in molar ratio as 1:(1~3)；Wherein, as bottom material
Cyclohexanone and surplus cyclohexanone molar ratio be 1:(1~3).By the cyclohexanone and surplus cyclohexanone that will be used as bottom material
Molar ratio limit within the above range, effectively reduce under reaction condition provided by the invention, n-butanal itself occur
The probability of condensation.
Further, according to the present invention, in the step of aldol reaction, the effect of the buck is to build
The reaction condition of alkalinity, the present invention do not have special requirement to it, can for well known to one of ordinary skill in the art, for example,
The buck is formulated using inorganic base and/or organic base, is specifically as follows alkali metal hydroxide, alkaline-earth metal hydrogen-oxygen
Compound, urea and its at least one of derivative and organic amine；It is further preferred that the buck be sodium hydroxide solution,
One of potassium hydroxide solution；It is further preferred that the mass fraction of the buck is 0.5%~5.0%.
In the present invention, the step of the aldol reaction in, control heating temperature is 50~100 DEG C, controls surplus
The time for adding of the mixture of cyclohexanone and n-butanal is 2~8h；It is added dropwise and ties in the mixture of surplus cyclohexanone and n-butanal
Shu Hou, is stirred and insulation reaction is detecting just then every the content of the n-butanal in half an hour detection primary first-order equation liquid
Reaction was completed when the content of butyraldehyde is below 1%, in general, the time of control insulation reaction is in 1~4h.In this way, may be implemented
Effective control to side reaction improves condensation reaction yield.
Further, according to the present invention, the specific steps of the hydrogenation reaction include: that will obtain after aldol reaction
The condensation product of bottom is added in high-pressure hydrogenation reaction kettle, and hydrogenation reaction solvent is added and Pd/C catalyst, room temperature add hydrogen extremely
Until not inhaling hydrogen, after distillation recovery hydrogenation reaction solvent is applied, intermediate product 2- butyl cyclohexanone is obtained.
Further, the hydrogenation pressure in the high-pressure hydrogenation reaction kettle is 0.1~1.0MPa.
In the present invention, the hydrogenation reaction solvent is selected from one of petroleum ether, hexamethylene, dichloroethanes.By with stone
The organic solvent of oily ether, hexamethylene or dichloroethanes as hydrogenation reaction, effectively overcomes and reacts endless in hydrogenation process
The shortcomings that complete and catalyst inactivates after applying, meanwhile, hydrogenation reaction solvent provided by the invention is also able to achieve solid-phase catalyst
With add being separately recovered for hydrogen solvent to apply.
In the present invention, the specific steps of the Baeyer-Villiger oxidation include: to be uniformly mixed acetic acid with hydrogen peroxide
It is prepared into spare after Peracetic acid, Peracetic acid is slowly dropped in intermediate product 2- butyl cyclohexanone, stirring to reaction knot
Beam；Water is added into the product after reaction, stirring is washed to neutrality, ε-decalactone is obtained after stratification.
Further, according to the present invention, the temperature of the Baeyer-Villiger oxidation reaction is controlled at 5~30 DEG C, instead
It is 2~12h between seasonable.
In technical solution provided by the invention, reacted by way of oxidant is added dropwise, it is ensured that oxidation reaction
Safety；In addition, by will acetic acid and hydrogen peroxide mix after be used as oxidant, compared to directlying adopt hydrogen peroxide as oxidant
Reaction condition, avoid the problem for bringing side reaction and oxidation time long.
In the present invention, the specific steps of the continuous hydrolyzing include: dropwise addition ε-decalactone in oxytropism solution, and side is added dropwise
While stirring to reaction terminates, stratification, oil reservoir is washed to neutrality, obtains milk lactone spice crude product；Milk lactone is fragrant
Material crude product is evaporated under reduced pressure to obtain final product milk lactone spice.
In actual specific operation process, it is added by acid solution head tank into the hydrolysis kettle of reaction and rectification device
Acid solution, turn on agitator and recirculated cooling water are added part ε-decalactone by ε-decalactone head tank, open steam valve
Then door and vacuum pump ε-decalactone are continuously added dropwise into hydrolysis kettle by ε-decalactone head tank, are had by hydrolysis kettle
Rectifying section collects distillate, obtains milk lactone crude product；Milk lactone crude product is washed to neutrality, and stratification separates water layer
To Sewage Disposal processing, collects oil reservoir and be evaporated under reduced pressure to product milk lactone synthetic perfume.By reacting lasting charging, from
And achievees the purpose that milk lactone spice and be continuously synthesizing to.
Further, according to the present invention, the acid solution is selected from one of sulfuric acid, phosphoric acid, hydrochloric acid；The acidity
The mass fraction of solution is 1.0%~50%.
Further, according to the present invention, the condition of the vacuum distillation include: control vacuum pressure be 667~
3333Pa, temperature are 135~160 DEG C.By the condition of the above-mentioned vacuum distillation of restriction, achieve the purpose that separating-purifying, it is made
The product obtained finally can satisfy the requirement of essence for food fragrance blending.
Below by way of specific embodiment to milk lactone spice provided by the invention be continuously synthesizing to method make into
The explanation of one step:
Embodiment 1
A kind of milk lactone spice is continuously synthesizing to method:
1) synthesis of 2- butylene pentylcyclohexanone
It is equipped in the 2000mL three-necked flask of thermometer, blender, dropping funel one, 1000mL mass fraction, which is added, is
2.5% sodium hydroxide solution, 98g cyclohexanone, turn on agitator after mixing, open thermostatic water bath, keep three-necked flask
Temperature is 75 DEG C, then the mixture of n-butanal 72g and cyclohexanone 98g is added dropwise into three-necked flask by dropping funel, and side is added dropwise
Side stirring, 2h is added dropwise, and continues thereafter with stirring, makes the above reactant the reaction was continued at 75 DEG C 2h, in detection reactant just
Reaction was completed when butyraldehyde content is lower than 1%.Cooling, stratification 2h；Water phase is applied to next group；Then by the above oil reservoir water
Washing is to neutrality, and liquid separation, vacuum distillation, the excessive cyclohexanone of collection, main distillate fraction are 2- butylene pentylcyclohexanone, and quality is referred to as
118.5g, yield 78.0%.
2) synthesis of 2- butyl cyclohexanone
2- butylene pentylcyclohexanone 100g and 5%Pd/C catalyst is added in the high-pressure hydrogenation reaction kettle with stirring rod
3g is replaced 5 times before being passed through hydrogen using nitrogen, using 200mL petroleum ether as hydrogenation reaction solvent then to high-pressure hydrogenation reaction kettle
It is inside passed through hydrogen, adds hydrogen until not inhaling hydrogen under the conditions of Yu Changwen, 0.4MPa, hydrogen is added to terminate using nitrogen displacement three times, then
Pd/C catalyst recovery is filtered out, reaction solution is transferred to distillation still, is distilled to recover petroleum ether and applies, obtains hydrogenation products 2- butyl
Cyclohexanone, weigh 100.1g, yield 98.8%.
3) preparation of peracetic acid
In 500mL three-necked flask, hydrogen peroxide and 300g acetic acid that 150g mass fraction is 50%, turn on agitator is added
And thermostatic water bath, it stirs evenly, concentrated sulfuric acid 13g is added dropwise under the conditions of 15 DEG C of temperature, stir 12h, it is spare to be prepared into Peracetic acid.
4) ε-decalactone synthesis
200g 2- butyl cyclohexanone is added in 1000mL three-necked flask, and Peracetic acid is added dropwise at 15~30 DEG C
460g, completion of dropwise addition stir 1h, add 300mL water, and organic layer is washed till neutrality with water by stratification 2h after stirring, dry
It is 220.2g, yield 98.7% that ε-decalactone crude product quality is obtained after organic layer.
5) synthesis of milk lactone
20g ε-decalactone crude product and 5g mass fraction 50% H is added in 250mL three-necked flask2SO4, control vacuum
Pressure be 1667Pa, be warming up to 140 DEG C；ε-decalactone crude product 200g is then persistently added dropwise thereto, collects distillate, warp
It washes, be evaporated under reduced pressure to product milk lactone 150g, yield 68%.
Experiment show:
1) detection of 2- butylene pentylcyclohexanone: product index of refraction is 1.4803 (literature values 1.4801)；Infared spectrum
(IR/cm-1) it is analyzed as follows: 2931.03,2862.33 (C-H), 1683.73 (C=O), 1449.67 (CH2), 1371.53
(CH3), 1608.22 (C=C) are almost the same with standard diagram, in conclusion product is determined as 2- butylene pentylcyclohexanone.
2) detection of 2- butyl cyclohexanone: product index of refraction is 1.4605 (literature values 1.4610)；Infared spectrum (IR/
cm-1) it is analyzed as follows: 2930.13,2859.32 (C-H), 1720.19 (C=O), 1444.98 (- CH2), 1269.63,1163.95
(C-O-C), consistent with standard diagram, product is determined as 2- butyl cyclohexanone.
3) 5 (6)-decylenic acid detection: product index of refraction is 1.4582 (literature value is 1.4520~1.4600)；Infrared figure
Compose (IR/cm-1) it is analyzed as follows: 3389.42,3360.23,2726.35,2665.34,1431.12 (O-H), 3087.03,
964.36 (=C-H), 2950.27,2928.01,2858.13,2865.16,1410.37 (C-H), 1702.35 (C=O),
1451.97(CH2), 1373.01 (CH3), 1278.38,1233.36 (C-O), consistent with standard spectrogram, product is determined as 5 (6)-
Decylenic acid；It is tested and analyzed by gas chromatograph-mass spectrometer, fraction relative molecular mass is 170.
Embodiment 2
Milk lactone spice as embodiment 1 provides is continuously synthesizing to method, unlike, in the conjunction of 5) milk lactone
Cheng Zhong, the pressure for controlling vacuum is 3333Pa, remaining condition is constant, and after measured, the yield of milk lactone is 60%.
Through analyzing, inventor's guess with the reduction of vacuum degree, necessarily improves the kettle temperature of rectifying still, in energy consumption
While, the temperature of fragrance product surface contact improves, and generates the bad miscellaneous gas being charred after bringing high-temperature coking, this and reality
The fragrance product being collected into has the characteristics that bad miscellaneous gas is consistent.
Comparative example 1
Milk lactone spice as embodiment 1 provides is continuously synthesizing to method, unlike, in the 2- cyclobutenyl
In the synthesis of cyclohexanone, it will be classified as at one as the cyclohexanone of bottom material and the surplus cyclohexanone mixed with n-butanal, it may be assumed that
It is equipped in the 2000mL three-necked flask of thermometer, blender, dropping funel one, 1000mL mass fraction, which is added, is
2.5% sodium hydroxide solution, turn on agitator after mixing, open thermostatic water bath, and keeping three-necked flask temperature is 75 DEG C,
The mixture of n-butanal 72g and cyclohexanone 196g is added dropwise into three-necked flask by dropping funel again, is stirred when being added dropwise, 2h drop
It adds complete；
Remaining condition is constant, after measured: the yield of 2- butylene pentylcyclohexanone is 70%.
Comparative example 2
Milk lactone spice as embodiment 1 provides is continuously synthesizing to method, unlike, in 4) ε-decalactone conjunction
" Peracetic acid " in embodiment 1 is changed to " hydrogen peroxide ", in dosage, application method and remaining preparation method by Cheng Zhong
It is constant, receive to obtain ε-decalactone crude product, after measured, yield 95.0%.
Basic principles and main features and the features of the present invention of the invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement is both fallen in the range of claimed invention.The scope of protection of present invention is by appended claims
And its equivalent thereof.
Claims (10)
1. a kind of milk lactone spice is continuously synthesizing to method, it is characterised in that: the synthetic method includes with n-butanal
It is raw material with cyclohexanone, aldol reaction is carried out under buck action condition, then hydrogenated reaction, Baeyer-
Villiger oxidation, most afterwards through sour continuous hydrolyzing, dehydration obtains the milk lactone spice；
The specific steps of the aldol reaction include: that the cyclohexanone by part as bottom material is uniformly mixed with buck, are heated
The mixture of surplus cyclohexanone and n-butanal is then added dropwise in processing, stirs when being added dropwise, and continue to stir after completion of dropwise addition
It mixes, reaction was completed below 1% for insulation reaction to the content for detecting n-butanal；
Oil reservoir is separated after standing, collects water layer and recovery；It collects oil reservoir and is transferred in distillation still after washing process and distilled
It recycles excessive cyclohexanone to apply, collects the condensation product of bottom.
2. milk lactone spice according to claim 1 is continuously synthesizing to method, it is characterised in that: the aldol condensation
In the step of reaction, the mass fraction of the buck is 0.5%~5.0%.
3. milk lactone spice according to claim 1 is continuously synthesizing to method, it is characterised in that: the aldol condensation
In the step of reaction, control heating temperature is 50~100 DEG C, when controlling the dropwise addition of the mixture of surplus cyclohexanone and n-butanal
Between be 2~8h.
4. milk lactone spice according to claim 1 is continuously synthesizing to method, it is characterised in that: the hydrogenation reaction
Specific steps include: that the condensation product of the bottom that will be obtained after aldol reaction is added in high-pressure hydrogenation reaction kettle, add
Enter hydrogenation reaction solvent and Pd/C catalyst, room temperature adds hydrogen until not inhaling hydrogen, after distillation recovery hydrogenation reaction solvent is applied, obtains
To intermediate product 2- butyl cyclohexanone.
5. milk lactone spice according to claim 4 is continuously synthesizing to method, it is characterised in that: the hydrogenation reaction
Solvent is selected from one of petroleum ether, hexamethylene, dichloroethanes.
6. milk lactone spice according to claim 1 is continuously synthesizing to method, it is characterised in that: the Baeyer-
Villiger oxidation specific steps include: acetic acid is uniformly mixed with hydrogen peroxide be prepared into Peracetic acid after it is spare, by peroxide
Acetic acid is slowly dropped in intermediate product 2- butyl cyclohexanone, and stirring to reaction terminates；Water is added into the product after reaction, stirs
It mixes and is washed to neutrality, ε-decalactone is obtained after stratification.
7. milk lactone spice according to claim 6 is continuously synthesizing to method, it is characterised in that: the Baeyer-
At 5~30 DEG C, the reaction time is 2~12h for the temperature control of Villiger oxidation reaction.
8. milk lactone spice according to claim 1 is continuously synthesizing to method, it is characterised in that: the serialization water
The specific steps of solution include: dropwise addition ε-decalactone in oxytropism solution, and stirring when being added dropwise to reaction terminates, stratification, oil
Layer is washed to neutrality, obtains milk lactone spice crude product；It is evaporated under reduced pressure milk lactone spice crude product to obtain final product ox
Milk lactone spice.
9. milk lactone spice according to claim 8 is continuously synthesizing to method, it is characterised in that: the acidity is molten
Liquid is selected from one of sulfuric acid, phosphoric acid, hydrochloric acid；
The mass fraction of the acid solution is 1.0%~50%.
10. milk lactone spice according to claim 8 is continuously synthesizing to method, it is characterised in that: the decompression is steamed
The condition evaporated includes: that the pressure of control vacuum is 667~3333Pa, and temperature is 135~160 DEG C.
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Cited By (3)
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| CN110128259A (en) * | 2019-06-12 | 2019-08-16 | 广东广益科技实业有限公司 | 5 (6)-decene acid production process |
| CN114075101A (en) * | 2020-08-20 | 2022-02-22 | 中国科学院大连化学物理研究所 | Preparation method of 2-alkyl cyclohexanone compound |
| CN114507123A (en) * | 2020-11-17 | 2022-05-17 | 中国科学院大连化学物理研究所 | Preparation method of 2-alkyl cyclohexanone homologue |
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| 曹永兴: "2-戊基环戊酮-3-乙酸甲酯的合成及其工艺研究", 《中国优秀硕士学位论文全文数据库（工程科技I辑）》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110128259A (en) * | 2019-06-12 | 2019-08-16 | 广东广益科技实业有限公司 | 5 (6)-decene acid production process |
| CN114075101A (en) * | 2020-08-20 | 2022-02-22 | 中国科学院大连化学物理研究所 | Preparation method of 2-alkyl cyclohexanone compound |
| CN114507123A (en) * | 2020-11-17 | 2022-05-17 | 中国科学院大连化学物理研究所 | Preparation method of 2-alkyl cyclohexanone homologue |
| CN114507123B (en) * | 2020-11-17 | 2023-10-10 | 中国科学院大连化学物理研究所 | Preparation method of 2-alkyl cyclohexanone homolog |
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