CN105399613B - A kind of preparation method of fragrance 6- methyl-3-heptene-2-ones - Google Patents
A kind of preparation method of fragrance 6- methyl-3-heptene-2-ones Download PDFInfo
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- CN105399613B CN105399613B CN201511013617.8A CN201511013617A CN105399613B CN 105399613 B CN105399613 B CN 105399613B CN 201511013617 A CN201511013617 A CN 201511013617A CN 105399613 B CN105399613 B CN 105399613B
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- 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
- C07C45/61—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups
- C07C45/67—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups by isomerisation; by change of size of the carbon skeleton
- C07C45/68—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups by isomerisation; by change of size of the carbon skeleton by increase in the number of carbon atoms
- C07C45/72—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups by isomerisation; by change of size of the carbon skeleton by increase in the number of carbon atoms by reaction of compounds containing >C = O groups with the same or other compounds containing >C = O groups
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Abstract
The present invention provides a kind of preparation method of 3 heptene of 6 methyl of fragrance, 2 ketone, including the dissolving of major catalyst and cocatalyst, addition solvent, addition acetone, dropwise addition isopentyl aldehyde.Product prepared by the present invention, overall yield is high, is 95.4 96.41% in terms of the total recovery of 2 two kinds of compounds of ketone of 6 methyl, 3 heptene, 2 ketone and 6 methyl, 4 enanthol；6 methyl, 3 heptene, 2 ketone content is 94.27 96.41%；6 methyl, 4 enanthol, 2 ketone content is 1.00 3.00%；The content that 6 methyl, 3 heptene, 2 ketone is obtained through rectifying reaches 99.10% or more；The conversion ratio of the high conversion rate of raw material, isopentyl aldehyde is 99.10 99.40%；Catalysis time is short, and catalysis time is 3.5 4.5 hours；Solvent of the present invention is easy to get using alkane solvents, factories such as hexamethylene, n-hexanes, is conducive to environmental protection, is reduced cost.
Description
Technical field
The present invention relates to a kind of preparation methods of 6- methyl-3-heptene-2-ones, especially to technique in preparation method and urge
The improvement of agent, belongs to technical field of chemical synthesis.
Background technology
6- methyl-3-heptene-2-ones are a kind of α, β-unsaturation methyl ketone, this kind of organic compound, pesticide,
Many aspects such as food additives are widely used and a kind of important flavor of raw material, and 6- methyl -3- hept- 2- ketone is
There is one new perfume material of newest announcement apples odorant, chemical property to stablize.Proline was as emerging catalysis in recent years
Agent is used for always α, the synthetic work of alpha, beta-unsaturated ketone compound.
In 2001《ORGANNIC LETEERS》Article in Vol.3, No.4《Proline-Catalyzed
Asymmetric Aldol Reactions between Ketones and r-Unsubstituted Aldehydes》It points out
At ambient temperature, it using DMSO as solvent, only using proline as catalyst, reacts 2-96 hours, 6- methyl -4- heptan can be obtained
Alcohol -2- ketone, selectivity 95%, but 6- methyl-3-heptene-2-ones can be obtained after its dehydration, it not yet mentions and how to carry out in article
Dehydration, has only carried out the synthetic work of back, and follow-up dewatering is not pointed out, while solvent is that DSMO industrialization is too expensive
Relatively it is difficult to realize.
In ACS Catalysis《Influence of the Organoctalyst in the Aldol/
Mannich-Type Product Selectivities in C-C Bond Forming Reactions》Article is pointed out with dried meat
Ammonia alcohol is catalyst, and at room temperature, catalysis reaction 24 hours can obtain 6- methyl-3-heptene-2-ones and 6- methyl -4- enanthol -2-
The mixture of ketone, wherein the ratio between 6- methyl -4- enanthol -2- ketone and 6- methyl-3-heptene-2-one contents are 60：10, and yield compared with
It is low, be not suitable for production and prepare 6- methyl-3-heptene-2-ones.
It to sum up uses proline or prolinol as catalyst in two documents, has the following deficiencies：
1, catalysis time is longer, that is, needs longer reaction time and dewatering time；
2, solvent DMSO is solvent, is unfavorable for environmental protection and the too high unsuitable large industrialized production of cost；
3, yield is relatively low, and there is no the precedent of industrial applications, 6- methyl -4- enanthol -2- ketone and 6- methyl -3- heptan
The ratio between alkene -2- ketone contents are 60：10, selectivity is poor, and feed stock conversion is low, is not suitable for production and prepares 6- methyl -3- heptene -2-
Ketone.
Invention content
To solve technical problem of the existing technology, the present invention provides a kind of preparation side of -3 hepten-2-one of 6- methyl
Method selects the inexpensive raw material isopentyl aldehyde being easily obtained and acetone to prepare -3 heptan of 6- methyl under the catalysis of alkaline composite catalyst
Alkene -2- ketone, to realize following goal of the invention：
（1）Product prepared by the present invention, overall yield is high, with 6- methyl-3-heptene-2-ones and 6- methyl -4- enanthol -2-
The total recovery meter of two kinds of compounds of ketone reaches 95.4-96.41%；
（2）After insulation reaction of the present invention in gained mixture, 6- methyl-3-heptene-2-one contents reach 94.27-
96.41%；6- methyl -4- enanthol -2- ketone contents are 1.00-3.00%；
（3）6- methyl-3-heptene-2-ones prepared by the present invention, product content is up to 99.10% or more after rectifying；
（4）The conversion ratio of preparation method of the present invention, the high conversion rate of raw material, isopentyl aldehyde reaches 99.10-99.40%；
（5）Preparation method of the present invention, catalysis time is short, and catalysis time is less than 5 hours；
（6）Solvent of the present invention is easy to get using alkane solvents, the factory such as hexamethylene, n-hexane, is conducive to environmental protection, reduce at
This.
In order to solve the above technical problems, the technical solution adopted by the present invention is as follows：
A kind of preparation method of fragrance 6- methyl-3-heptene-2-ones, it is characterised in that：Including major catalyst and auxiliary catalysis
The dissolving of agent is added solvent, acetone is added, isopentyl aldehyde is added dropwise.
It is to be further improved to above-mentioned technical proposal below：
The major catalyst is prolinol；The cocatalyst is secondary amine or tertiary amine.
The cocatalyst is one or more in di-n-propylamine, di-n-butylamine, trimethylamine.
The molar ratio of the major catalyst and cocatalyst is 0.1-1.
The molar ratio of the major catalyst and cocatalyst, preferably 0.1-0.5.
The dissolving of the major catalyst and cocatalyst, using water dissolution major catalyst, cocatalyst；The dosage of the water
Molar ratio with isopentyl aldehyde is 10-30, preferably 10-15.
The dropwise addition isopentyl aldehyde, isopentyl aldehyde and the molar ratio of major catalyst prolinol are：7-20；The dropwise addition of the isopentyl aldehyde
Time is 1-10 hours.
The dropwise addition isopentyl aldehyde, the molar ratio of isopentyl aldehyde and major catalyst prolinol, preferably 7-10；The isopentyl aldehyde
Time for adding is preferably 2-4 hours.
The molar ratio of the addition acetone, isopentyl aldehyde and acetone is 0.2-2, preferably 0.5-1.0；
The molar ratio of the addition solvent, isopentyl aldehyde and solvent is：0.1-0.7, preferably 0.28-0.46.
The solvent is alkane solvent；The alkane solvent is hexamethylene, one or more in toluene, n-hexane；
The isopentyl aldehyde is reacted under acetone in the presence of water composite catalyst catalysis, and 0-60 DEG C of reaction temperature preferably exists
10-50℃。
The feed way of raw material is to be firstly added major catalyst prolinol, water during isopentyl aldehyde is reacted with acetone in the above method
And cocatalyst is mixed to being completely dissolved, and alkane solvents are then added, and is added after acetone is warming up to required temperature and is added dropwise
Isopentyl aldehyde.
In the mixture for reacting gained with acetone according to isopentyl aldehyde of the present invention, the usual 6- methyl-of content containing 1.00%-3.00%
4- enanthol -2- ketone, but subsequent processing work is not influenced.
Compared with prior art, beneficial effects of the present invention are：
The present invention is had the following advantages compared with prior art using above technical scheme：
（1）Product prepared by the present invention, overall yield is high, with 6- methyl-3-heptene-2-ones and 6- methyl -4- enanthol -2-
The total recovery meter of two kinds of compounds of ketone is 95.4-96.41%；
（2）After insulation reaction of the present invention in gained mixture, 6- methyl-3-heptene-2-one contents are 94.27-
96.41%；6- methyl -4- enanthol -2- ketone contents are 1.00-3.00%；
（3）6- methyl-3-heptene-2-ones prepared by the present invention, product 6- methyl-3-heptene-2-one contents are after rectifying
99.2-99.55%；
（4）The conversion ratio of preparation method of the present invention, the high conversion rate of raw material, isopentyl aldehyde is 99.1-99.40%；
（5）Preparation method of the present invention, catalysis time is short, and catalysis time is 3.5-4.5 hours；
（6）Solvent of the present invention is easy to get using alkane solvents, the factory such as hexamethylene, n-hexane, is conducive to environmental protection, reduce at
This.
Specific implementation mode
Hereinafter, preferred embodiments of the present invention will be described, it should be understood that preferred embodiment described herein is only used
In the description and interpretation present invention, it is not intended to limit the present invention.
A kind of preparation method of 1 fragrance 6- methyl-3-heptene-2-ones of embodiment
Include the following steps：
（1）The dissolving of major catalyst and cocatalyst
By 10.1g（0.1mol）Prolinol, water 180g (10mol), di-n-butylamine 12.02g (0.1mol) mixing are put into
It is cooling in 1000ml four-hole boiling flasks, stirring；
（2）Solvent is added
Solvent hexamethylene 300g (3.57mol) is added；
（3）Acetone is added
Add acetone 58g（1mol）；
（4）Isopentyl aldehyde is added dropwise
Etc. cooling to 10 DEG C, start that isopentyl aldehyde 86g is added dropwise（1mol）, time for adding is 2 hours；
（5）Insulation reaction
After completion of dropwise addition, insulation reaction 1.5 hours to gas phase analysis isoamyl aldehyde is less than 0.60%；In reaction mixture
- 3 hepten-2-one of gas phase analysis 6- methyl is more than 96.00% with the total ketone content of 6- methyl -4- enanthol -2- ketone；
（6）Rectifying
Divide and go water phase, obtains organic phase, recycling design, rectifying obtains the yellowish liquid 6- methyl-3-heptene-2-ones of product and 6-
Methyl -4- enanthol -2- two kinds of compound 120.96g of ketone, wherein -3 hepten-2-one 117.33g of 6- methyl, content 99.50%,
It is calculated as 96.00% with the total recovery of 6- methyl-3-heptene-2-ones and 6- methyl -4- enanthol -2- two kinds of compounds of ketone, isopentyl aldehyde
Conversion ratio is 99.31%.
A kind of preparation method of 2 fragrance 6- methyl-3-heptene-2-ones of embodiment
Include the following steps：
（1）The dissolving of major catalyst and cocatalyst
By 10.1g（0.1mol）Prolinol, water 180g (10mol), di-n-butylamine 12.02g (0.1mol) mixing are put into
In 1000ml four-hole boiling flasks, stirring；
（2）Solvent is added
Solvent hexane 300g (3.49mol) is added；
（3）Acetone is added
Add acetone 58g（1mol）；
（4）Isopentyl aldehyde is added dropwise
30 DEG C are warming up to, starts that isopentyl aldehyde 86g is added dropwise（1mol）, time for adding is 3 hours；
（5）Insulation reaction
After completion of dropwise addition, insulation reaction 1.0 hours to gas phase analysis isoamyl aldehyde is less than 0.70%；In reaction mixture
- 3 hepten-2-one of gas phase analysis 6- methyl is more than 96.00% with the total ketone content of 6- methyl -4- enanthol -2- ketone；
（6）Rectifying
Divide and go water phase, obtains organic phase, recycling design, rectifying obtains the yellowish liquid 6- methyl-3-heptene-2-ones of product and 6-
Methyl -4- enanthol -2- two kinds of compound 120.71g of ketone, wherein -3 hepten-2-one 116.84g of 6- methyl, content 99.43%,
It is calculated as 95.80% with the total recovery of 6- methyl-3-heptene-2-ones and 6- methyl -4- enanthol -2- two kinds of compounds of ketone, isopentyl aldehyde
Conversion ratio is 99.25%.
A kind of preparation method of 3 fragrance 6- methyl-3-heptene-2-ones of embodiment
Include the following steps：
（1）The dissolving of major catalyst and cocatalyst
By 10.1g（0.1mol）Prolinol, water 180g (10mol), di-n-butylamine 12.02g (0.1mol) mixing are put into
In 1000ml four-hole boiling flasks, stirring；
（2）Solvent is added
Solvent toluene 400g (4.32mol) is added；
（3）Acetone is added
Add acetone 58g（1mol）；
（4）Isopentyl aldehyde is added dropwise
50 DEG C are warming up to, starts that isopentyl aldehyde 86g is added dropwise（1mol）, time for adding is 4 hours；
（5）Insulation reaction
After completion of dropwise addition, insulation reaction 0.5 hour to gas phase analysis isoamyl aldehyde is less than 0.60%；In reaction mixture
- 3 hepten-2-one of gas phase analysis 6- methyl is more than 96.00% with the total ketone content of 6- methyl -4- enanthol -2- ketone；
（6）Rectifying
Divide and go water phase, obtains organic phase, recycling design, rectifying obtains the yellowish liquid 6- methyl-3-heptene-2-ones of product and 6-
Methyl -4- enanthol -2- two kinds of compound 121.21g of ketone, wherein -3 hepten-2-one 116.97g of 6- methyl, content 99.45%,
It is calculated as 96.20% with the total recovery of 6- methyl-3-heptene-2-ones and 6- methyl -4- enanthol -2- two kinds of compounds of ketone, isopentyl aldehyde
Conversion ratio is 99.35%.
A kind of preparation method of 4 fragrance 6- methyl-3-heptene-2-ones of embodiment
Include the following steps：
（1）The dissolving of major catalyst and cocatalyst
By 21.21g（0.21mol）Prolinol, water 300g (16.67mol), trimethylamine 20.69g (0.35mol) mixing are put
Enter in 2000ml four-hole boiling flasks, cooling, stirring；
（2）Solvent is added
Solvent hexamethylene 300g (3.57mol) is added；
（3）Acetone is added
Add acetone 116g（2mol）；
（4）Isopentyl aldehyde is added dropwise
Etc. cooling to 10 DEG C, start that isopentyl aldehyde 129g is added dropwise（1.5mol）, time for adding is 2 hours；
（5）Insulation reaction
After completion of dropwise addition, insulation reaction 2.0 hours to gas phase analysis isoamyl aldehyde is less than 0.80%；In reaction mixture
- 3 hepten-2-one of gas phase analysis 6- methyl is more than 96.00% with the total ketone content of 6- methyl -4- enanthol -2- ketone；
（6）Rectifying
Divide and go water phase, obtains organic phase, recycling design, rectifying obtains the yellowish liquid 6- methyl-3-heptene-2-ones of product and 6-
Methyl -4- enanthol -2- two kinds of compound 180.30g of ketone, wherein -3 hepten-2-one 174.90g of 6- methyl, content 99.20%,
It is calculated as 95.40% with the total recovery of 6- methyl-3-heptene-2-ones and 6- methyl -4- enanthol -2- two kinds of compounds of ketone, isopentyl aldehyde
Conversion ratio is 99.19%.
A kind of preparation method of 5 fragrance 6- methyl-3-heptene-2-ones of embodiment
Include the following steps：
（1）The dissolving of major catalyst and cocatalyst
By 21.21g（0.21mol）Prolinol, water 300g (16.67mol), trimethylamine 20.69g (0.35mol) mixing are put
Enter in 2000ml four-hole boiling flasks, stirs；
（2）Solvent is added
Solvent hexane 300g (3.49mol) is added；
（3）Acetone is added
Add acetone 116g（2mol）；
（4）Isopentyl aldehyde is added dropwise
30 DEG C are warming up to, starts that isopentyl aldehyde 129g is added dropwise（1.5mol）, time for adding is 3 hours；
（5）Insulation reaction
After completion of dropwise addition, insulation reaction 1.0 hours to gas phase analysis isoamyl aldehyde is less than 0.70%；In reaction mixture
- 3 hepten-2-one of gas phase analysis 6- methyl is more than 96.00% with the total ketone content of 6- methyl -4- enanthol -2- ketone；
（6）Rectifying
Divide and go water phase, obtains organic phase, recycling design, rectifying obtains the yellowish liquid 6- methyl-3-heptene-2-ones of product and 6-
Methyl -4- enanthol -2- two kinds of compound 181.33g of ketone, wherein -3 hepten-2-one 174.61g of 6- methyl, content 99.50%,
It is calculated as 95.94% with the total recovery of 6- methyl-3-heptene-2-ones and 6- methyl -4- enanthol -2- two kinds of compounds of ketone, isopentyl aldehyde
Conversion ratio is 99.22%.
A kind of preparation method of 6 fragrance 6- methyl-3-heptene-2-ones of embodiment
Include the following steps：
（1）The dissolving of major catalyst and cocatalyst
By 21.21g（0.21mol）Prolinol, water 300g (16.67mol), trimethylamine 20.69g (0.35mol) mixing are put
Enter in 2000ml four-hole boiling flasks, stirs；
（2）Solvent is added
Solvent toluene 400g (4.32mol) is added；
（3）Acetone is added
Add acetone 116g（2mol）；
（4）Isopentyl aldehyde is added dropwise
50 DEG C are warming up to, starts that isopentyl aldehyde 129g is added dropwise（1.5mol）, time for adding is 4 hours；
（5）Insulation reaction
After completion of dropwise addition, insulation reaction 0.5 hour to gas phase analysis isoamyl aldehyde is less than 0.60%；In reaction mixture
- 3 hepten-2-one of gas phase analysis 6- methyl is more than 96.00% with the total ketone content of 6- methyl -4- enanthol -2- ketone；
（6）Rectifying
Divide and go water phase, obtains organic phase, recycling design, rectifying obtains the yellowish liquid 6- methyl-3-heptene-2-ones of product and 6-
Methyl -4- enanthol -2- two kinds of compound 181.63g of ketone, wherein -3 hepten-2-one 175.64g of 6- methyl, content 99.41%,
It is calculated as 96.10% with the total recovery of 6- methyl-3-heptene-2-ones and 6- methyl -4- enanthol -2- two kinds of compounds of ketone, isopentyl aldehyde
Conversion ratio is 99.32%.
A kind of preparation method of 7 fragrance 6- methyl-3-heptene-2-ones of embodiment
Include the following steps：
（1）The dissolving of major catalyst and cocatalyst
By 17.17g（0.17mol）Prolinol, water 600g (16.67mol), trimethylamine 20.69g (0.35mol) mixing are put
Enter in 2000ml four-hole boiling flasks, stirs；
（2）Solvent is added
Solvent toluene 400g (4.32mol) is added；
（3）Acetone is added
Add acetone 232g（4mol）；
（4）Isopentyl aldehyde is added dropwise
50 DEG C are warming up to, starts that isopentyl aldehyde 172g is added dropwise（2mol）, time for adding is 2 hours；
（5）Insulation reaction
After completion of dropwise addition, insulation reaction 2.0 hours to gas phase analysis isoamyl aldehyde is less than 0.70%；In reaction mixture
- 3 hepten-2-one of gas phase analysis 6- methyl is more than 96.00% with the total ketone content of 6- methyl -4- enanthol -2- ketone；
（6）Rectifying
Divide and go water phase, obtains organic phase, recycling design, rectifying obtains the yellowish liquid 6- methyl-3-heptene-2-ones of product and 6-
Methyl -4- enanthol -2- two kinds of compound 181.87g of ketone, wherein -3 hepten-2-one 174.78g of 6- methyl, content 99.35%,
It is calculated as 96.23% with the total recovery of 6- methyl-3-heptene-2-ones and 6- methyl -4- enanthol -2- two kinds of compounds of ketone, isopentyl aldehyde
Conversion ratio is 99.22%.
A kind of preparation method of 8 fragrance 6- methyl-3-heptene-2-ones of embodiment
Include the following steps：
（1）The dissolving of major catalyst and cocatalyst
By 10.1g（0.1mol）Prolinol, water 270g (15mol), di-n-propylamine 101.19g (1mol) mixing are put into
It is cooling in 2000ml four-hole boiling flasks, stirring；
（2）Solvent is added
Solvent hexamethylene 840g (10mol) is added；
（3）Acetone is added
Add acetone 58g（1mol）；
（4）Isopentyl aldehyde is added dropwise
Etc. cooling to 10 DEG C, start that isopentyl aldehyde 86g is added dropwise（1mol）, time for adding is 2 hours；
（5）Insulation reaction
After completion of dropwise addition, insulation reaction 2.0 hours to gas phase analysis isoamyl aldehyde is less than 0.70%；In reaction mixture
- 3 hepten-2-one of gas phase analysis 6- methyl is more than 96.00% with the total ketone content of 6- methyl -4- enanthol -2- ketone；
（6）Rectifying
Divide and go water phase, obtains organic phase, recycling design, rectifying obtains the yellowish liquid 6- methyl-3-heptene-2-ones of product and 6-
Methyl -4- enanthol -2- two kinds of compound 121.31g of ketone, wherein -3 hepten-2-one 117.67g of 6- methyl, content 99.45%,
It is calculated as 96.28% with the total recovery of 6- methyl-3-heptene-2-ones and 6- methyl -4- enanthol -2- two kinds of compounds of ketone, isopentyl aldehyde
Conversion ratio is 99.28%.
A kind of preparation method of 9 fragrance 6- methyl-3-heptene-2-ones of embodiment
Include the following steps：
（1）The dissolving of major catalyst and cocatalyst
By 10.1g（0.1mol）Prolinol, water 540g (30mol), di-n-propylamine 101.19g (1mol) mixing are put into
It is cooling in 1000ml four-hole boiling flasks, stirring；
（2）Solvent is added
Solvent toluene 248.4g (2.70mol) is added；
（3）Acetone is added
Add acetone 58g（1mol）；
（4）Isopentyl aldehyde is added dropwise
Etc. cooling to 10 DEG C, start that isopentyl aldehyde 86g is added dropwise（1mol）, time for adding is 2 hours；
（5）Insulation reaction
After completion of dropwise addition, insulation reaction 2.0 hours to gas phase analysis isoamyl aldehyde is less than 0.60%；In reaction mixture
- 3 hepten-2-one of gas phase analysis 6- methyl is more than 96.00% with the total ketone content of 6- methyl -4- enanthol -2- ketone；
（6）Rectifying
Divide and go water phase, obtains organic phase, recycling design, rectifying obtains the yellowish liquid 6- methyl-3-heptene-2-ones of product and 6-
Methyl -4- enanthol -2- two kinds of compound 121.44g of ketone, wherein -3 hepten-2-one 116.82g of 6- methyl, content 99.55%,
It is calculated as 96.38% with the total recovery of 6- methyl-3-heptene-2-ones and 6- methyl -4- enanthol -2- two kinds of compounds of ketone, isopentyl aldehyde
Conversion ratio is 99.38%.
A kind of preparation method of 10 fragrance 6- methyl-3-heptene-2-ones of embodiment
Include the following steps：
（1）The dissolving of major catalyst and cocatalyst
By 10.1g（0.1mol）Prolinol, water 540g (30mol), di-n-propylamine 101.19g (1mol) mixing are put into
It is cooling in 1000ml four-hole boiling flasks, stirring；
（2）Solvent is added
Solvent hexane 123.23g (1.43mol) is added；
（3）Acetone is added
Add acetone 58g（1mol）；
（4）Isopentyl aldehyde is added dropwise
Etc. cooling to 10 DEG C, start that isopentyl aldehyde 86g is added dropwise（1mol）, time for adding is 2 hours；
（5）Insulation reaction
After completion of dropwise addition, insulation reaction 2.0 hours to gas phase analysis isoamyl aldehyde is less than 0.60%；In reaction mixture
- 3 hepten-2-one of gas phase analysis 6- methyl is more than 96.00% with the total ketone content of 6- methyl -4- enanthol -2- ketone；
（6）Rectifying
Divide and go water phase, obtains organic phase, recycling design, rectifying obtains the yellowish liquid 6- methyl-3-heptene-2-ones of product and 6-
Methyl -4- enanthol -2- two kinds of compound 121.30g of ketone, wherein -3 hepten-2-one 117.05g of 6- methyl, content 99.41%,
It is calculated as 96.27% with the total recovery of 6- methyl-3-heptene-2-ones and 6- methyl -4- enanthol -2- two kinds of compounds of ketone, isopentyl aldehyde
Conversion ratio is 99.30%.
Unless otherwise indicated, the percentage employed in the present invention is weight percent, ratio of the present invention,
For mass ratio.
Finally it should be noted that：The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
With technical scheme described in the above embodiments is modified or equivalent replacement of some of the technical features.
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in the present invention's
Within protection domain.
Claims (4)
1. a kind of preparation method of fragrance 6- methyl-3-heptene-2-ones, it is characterised in that：Including major catalyst and cocatalyst
Dissolving, be added solvent, be added acetone, be added dropwise isopentyl aldehyde；
The major catalyst is prolinol；The cocatalyst is secondary amine or tertiary amine；The major catalyst and cocatalyst
Molar ratio, be 0.1-0.5；
The secondary amine or tertiary amine are one or more in di-n-propylamine, di-n-butylamine, trimethylamine；
The solvent is hexamethylene, n-hexane or toluene；
The isopentyl aldehyde and the molar ratio of major catalyst prolinol are：7-20；
The molar ratio of the addition acetone, isopentyl aldehyde and acetone is 0.2-2；
Reaction temperature is 0-60 DEG C；
The dissolving of the major catalyst and cocatalyst, using water dissolution major catalyst, cocatalyst；The dosage of the water with it is different
The molar ratio of valeral is 10-30.
2. a kind of preparation method of fragrance 6- methyl-3-heptene-2-ones according to claim 1, it is characterised in that：Institute
Dropwise addition isopentyl aldehyde is stated, the time for adding of the isopentyl aldehyde is 1-10 hours.
3. a kind of preparation method of fragrance 6- methyl-3-heptene-2-ones according to claim 2, it is characterised in that：It is described
Isopentyl aldehyde, the molar ratio of isopentyl aldehyde and major catalyst prolinol, preferably 7-10 is added dropwise；The time for adding of the isopentyl aldehyde is preferred
It is 2-4 hours.
4. a kind of preparation method of fragrance 6- methyl-3-heptene-2-ones according to claim 1, it is characterised in that：It is described
Solvent is added, the molar ratio of isopentyl aldehyde and solvent is：0.1-0.7.
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