CN108586420A - A kind of green synthesis process of Jiale muskiness - Google Patents
A kind of green synthesis process of Jiale muskiness Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/94—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems condensed with rings other than six-membered or with ring systems containing such rings
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
Abstract
The present invention relates to a kind of green synthesis process of Jiale muskiness, in preparing intermediate pentamethyl indane, sulfonic acid type storng-acid cation exchange resin prepared by the present invention is selected to be reacted under solvent-free conditions as catalyst, " three wastes " pollution can be reduced, solid catalysis, which is easily isolated, is conducive to industrialized production, and yield is up to 70% or more.
Description
Technical field
The present invention relates to organic chemical industries to synthesize field, and in particular to a kind of green synthesis process of Jiale muskiness.
Background technology
Natural musk source is few, is not easy to obtain, the sachet of the male musk deer deer of per kilogram Moschus needs 60, and the current whole world
The annual output of natural musk is about 350k (content 70%).With disturbed ecological balance, the resource of natural musk is increasingly deficient.By
It is catched and killed in the deterioration of ecological environment and excess, the wild musk deer stock number in China is drastically reduced, and on-hand quantity is less than 20 middle of century
When l/10.For this purpose, the domestic musk deer in China is just classified as animals under first-class state protection in the 1980s, forbid to carry out any
Form is caught.People attempt to take perfume (or spice) using live body by artificial feeding musk deer deer to obtain Moschus, due to the property of male musk deer deer
Lattice are irascible, and sachet is the object of their indispensability again, and male musk deer is often dead after taking perfume (or spice).Years of researches the result shows that, manually
Raising live body takes perfume also to can not receive ideal effect.Growing with the demand of Moschus, natural musk is far from meeting work
The demand of industry, resource critical shortage, the price is very expensive, is above very limited in application.Therefore development musk ambrette be must
Right development trend.
Jiale muskiness is a kind of tricyclic iso-chroman type Moschus that the chemist of IFF companies of the U.S. is successfully synthesized first,
And patent was obtained in 1962.Jiale muskiness (Galaxolide) is a kind of widely applied Moschus type synthetic perfume, it is certainly
It is not present in right boundary.It is colourless highly viscous liquid, is dissolvable in water in ethyl alcohol and oil, not soluble in water.Its chemical constitution is as follows：
Molecular formula is C18H260, molecular weight 258.4, chemical name：L, 2,3,4,6,7,8- hexahydro -4,6,6,7,8,8--
Hexamethyl-γ -2- chromenes.Appearance is the thick liquid of water white transparency.
Jiale muskiness itself has the musk odor of height, and odor type is graceful, and fragrance is sweet, has an effect thoroughly and extension is splendid,
Lasting is lasting, and stability is good, is usually used in cosmetic cream, toner, soap and daily essence, tobacco essence, food flavor, prepares
Cosmetic essence and fixastive etc. as essence and flavoring agent deodorant tune.Since the musk odor of the product is strong, stability is good, nothing
Poison will not be absorbed by human body viscera, can be taken orally, and price is again cheaper, thus Jiale muskiness is liked by perfumer deeply
Love.The gesture of substituted dimethyl benzene Moschus and nitro musk has been presented in Jiale muskiness, is kind promising in polycyclic musk.
Existing production technology is that α-methylstyrene (AMS) and tert-pentyl alcohol carry out condensation reaction, the product pentamethyl of generation
With propylene oxide hydroxyl isopropylation occurs for indane, and chloromethyl etherificate occurs with polyformaldehyde for the hexamethyl indanol of generation instead again
Ying Hou, last condensation and cyclization, obtains Jiale muskiness.The technique uses second acid as catalyst during preparing indane, at waste liquid
Reason difficulty, seriously polluted, yield 48%；Making needs during each indanol to use excessive pentamethyl indane as raw material and molten
Agent, cost is higher, relatively low yield is only 48%；Also useful chlorobenzene does solvent, yield 58.4%, but the toxicity of chlorobenzene is big,
Influence the application range of product；It prepares Jiale muskiness and uses hydrogen chloride gas in the process, and react generation severe toxicity pair with polyformaldehyde
Product chloromethyl ether, yield 90%.
To the green synthesis process skill of Jiale muskiness, that there are yields is low, and liquid waste processing is difficult, cost is higher etc. for report at present
Disadvantage, the present invention in view of the deficiencies of the prior art, by selecting better catalysts and solvents, improve prior art, reduce " three
It is useless " pollution and equipment etching problem, while improving yield, reducing cost.
Invention content
To solve the above problems, the present invention provides a kind of green synthesis process of Jiale muskiness, include the following steps：
(1) pentamethyl indane is synthesized
Tert-pentyl alcohol and sulfonic acid type storng-acid cation exchange resin are added in reactor, then while stirring to reactor
Middle dropwise addition α-methylstyrene；Mixing speed and drop speed are controlled, is reacted 3~10 hours；Material after reaction through standing, being layered,
It is recycling to filter to isolate sulfonic acid type strong acid cation exchange resin catalyst, organic phase detaches unreacted original through rectifying
Material obtains indane；
(2) hexamethyl indanol is synthesized
Pentamethyl indane and organic solvent are added in reactor, are added at being -15~-10 DEG C in temperature anhydrous
ZnCl2, and turn on agitator, it is slowly added to propylene oxide solution after stirring a period of time, after the reaction was continued 5~10 hours, is added
Enter in mixture of ice and water, be sufficiently stirred, stand, be layered, isolates lower layer's organic phase；Organic phase 10%NaOH solution, saturation
Saline solution and deionized water are washed in turn, are washed till neutrality, obtain thick indanol；It is light that thick indanol is moved into progress rectifying in flask
The sticky oily liquids of yellow, i.e. indanol；
(3) Jiale muskiness is synthesized
Indanol and organic solvent are added in reactor, phosphorus pentachloride is then slowly added into, continues stirring 20~30
Minute, metaformaldehyde is added, is warming up at 50~60 DEG C and deionized water is added dropwise, reacts 3~5 hours, liquid separation takes organic phase to add again
It is that 10%NaOH carries out alkali cyclization 1~3 hour to enter mass concentration, and liquid separation again obtains organic phase, is obtained after rectifying thick
Jiale muskiness handles to have the Jiale muskiness of strong muskiness at 50 DEG C with ethyl alcohol recrystallization.
It in step 1), reacts for solvent-free reaction, the temperature of reaction is 30~50 DEG C, tert-pentyl alcohol and α-methylstyrene
Molar ratio be 1:1~2:1, the dosage of catalyst is the 1~10% of tert-pentyl alcohol quality.The catalyst is sulfonic acid type highly acid
Cation exchange resin, it is characterised in that：Include the following steps,
(1) it is by acrylic compounds ethylene oxidic ester, the mixture solution of the mixture of divinylbenzene and initiator and pH
Suspension polymerization is carried out after the aqueous solution mixing of 10~12 hydrosol, obtains bead cross-linked copolymer skeleton.
(2) the bead cross-linked copolymer skeleton obtained in step (1), the aqueous solution of sulfamate and sweller is mixed
It closes, the sulfonic acid type storng-acid cation exchange resin is obtained by the reaction under being 8~12 in pH.
The temperature of the polymerisation is 75~90 DEG C, and the reaction time is 3~5 hours.The hydrosol is selected from gelatin, hydroxyl
Methylcellulose, polyvinyl alcohol and combination thereof, dosage are 0.65~0.7% weight of oil phase raw material, aqueous solution
0.5%~5% weight of concentration.The initiator is dibenzoyl peroxide or azodiisobutyronitrile, accounts for oil phase raw material
0.15~0.2% weight.
The wherein described sweller is dichloroethanes or N, N- diformazan subunit formamides, bead crosslinked resin skeleton with it is molten
Swollen dose of weight ratio is 1:2~1:4；And the sulfamate be sylvite or sodium salt, the aqueous solution of the sulfamate
A concentration of 5~15% weight.
In preparing intermediate pentamethyl indane, sulfonic acid type storng-acid cation exchange resin prepared by the selection present invention is made
It is reacted under solvent-free conditions for catalyst, it is possible to reduce " three wastes " pollute, and solid catalysis, which is easily isolated, is conducive to industrial metaplasia
Production, yield are up to 70% or more.
In step 2), organic solvent be selected from dichloromethane, 1,2- dichloroethanes, chlorobenzene equal solvent, pentamethyl indane with
The molar ratio of propylene oxide is 1:5~1:10；The dosage of aluminum trichloride (anhydrous) is pentamethyl indane 1~5 (mol) %.
In step 3), organic solvent is selected from tetrahydrofuran, dichloromethane, 1,2- dichloroethanes etc.；Indanol and pentachloro-
The molar ratio for changing phosphorus is 1:1.2~1:1.5；The molar ratio of metaformaldehyde and indanol is 1:1~1:2；Synthesizing good happy musk deer
It in perfume (or spice), selects phosphorus pentachloride as catalyst, can improve and equipment be corroded in production process and to staff's actual bodily harm
The problem of, yield is improved, yield is up to 98% or more.
By adopting the above-described technical solution, the beneficial effects of the invention are as follows：
1, in preparing intermediate pentamethyl indane, the selection sulfonic acid type storng-acid cation exchange resin of the invention prepared
It is reacted under solvent-free conditions as catalyst, it is possible to reduce " three wastes " pollute, and solid catalysis, which is easily isolated, to be conducive to industrialize
Production, yield are up to 70% or more.
2, it in synthesizing Jiale muskiness, selects phosphorus pentachloride as catalyst, can improve in production process to equipment corruption
Erosion and the problem of to staff's actual bodily harm, improves yield, yield is up to 98% or more.
Specific implementation mode
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, the every other embodiment that those of ordinary skill in the art are obtained without making creative work,
It shall fall within the protection scope of the present invention.
【Embodiment 1】
Sulfonic acid type storng-acid cation exchange resin, preparation method includes the following steps,
(1) 0.25g gelatin is put into be equipped with and is gone in the four-hole boiling flask of 60.0g ionized waters, stirring is warming up to 45 DEG C, works as gelatin
0.025g hydroxymethyl celluloses are added after dissolving, the pH of water phase is adjusted to 10 with 5%NaOH aqueous solutions and 5% boric acid aqueous solution and is obtained
Obtain hydrosol solution.18g glycidyl methacrylate and 8.7g divinylbenzenes is added in 0.5g dibenzoyl peroxides
It in mixed liquor, is added in above-mentioned hydrosol solution and carries out suspension polymerization, obtain bead cross-linked copolymer skeleton 53g.
(2) it is 15% the bead cross-linked copolymer skeleton 10g obtained in step (1) to be added to 50mL mass concentrations
In N- diformazan subunit formamides, the sulfonic acid type strong acid is obtained by the reaction under being 8~12 in pH in sulfamic acid sodium water solution and 30gN
Property cation exchange resin.
【Embodiment 2】
Sulfonic acid type storng-acid cation exchange resin, preparation method includes the following steps,
(1) 0.35g gelatin is put into be equipped with and is gone in the four-hole boiling flask of 60.0g ionized waters, stirring is warming up to 45 DEG C, works as gelatin
0.025g hydroxymethyl celluloses are added after dissolving, the pH of water phase is adjusted to 11 with 5%NaOH aqueous solutions and 5% boric acid aqueous solution and is obtained
Obtain hydrosol solution.20.0g glycidyl methacrylate and 12g divinylbenzenes is added in 0.8g dibenzoyl peroxides
It in mixed liquor, is added in above-mentioned hydrosol solution and carries out suspension polymerization, obtain bead cross-linked copolymer skeleton 25g.
(2) it is 17% the bead cross-linked copolymer skeleton 15g obtained in step (1) to be added to 60mL mass concentrations
In N- diformazan subunit formamides, the sulfonic acid type strong acid is obtained by the reaction under being 8~12 in pH in sulfamic acid sodium water solution and 42gN
Property cation exchange resin.
【Embodiment 3】
(1) pentamethyl indane is synthesized
Sulfonic acid type storng-acid cation exchange resin 5.6g prepared by tert-pentyl alcohol 88g and embodiment 1 is added in reactor,
α-methylstyrene 100g is added dropwise into reactor while stirring again；Mixing speed and drop speed are controlled, it is small that 10 are reacted at 40 DEG C
When.For material after reaction through standing, being layered, filtering to isolate sulfonic acid type strong acid cation exchange resin catalyst can be sharp again
With organic phase detaches unreacted raw material through rectifying and obtains indane 123.2g, yield 72.8%；
(2) hexamethyl indanol is synthesized
Pentamethyl indane 18.8g and 100mL dichloromethane is added in reactor, nothing is added at being -15 DEG C in temperature
Water 1.3g ZnCl2, and turn on agitator, the 30mL dichloromethane that 29g propylene oxide is slowly added to after stirring a period of time are molten
Liquid after the reaction was continued 10 hours, is added in mixture of ice and water, is sufficiently stirred, stands, be layered, isolate lower layer's organic phase.It is organic
It is mutually washed in turn with 10%NaOH solution, saturated salt solution and deionized water, is washed till neutrality, is dried to obtain thick indanol.It will be thick
Indanol, which moves into, carries out the faint yellow sticky oily liquids 20g of rectifying, i.e. indanol in flask.
(3) Jiale muskiness is synthesized
Indanol 12.3g and dichloromethane 100mL are added in reactor, phosphorus pentachloride is then slowly added into
24.96g continues stirring 30 minutes, and metaformaldehyde 9.9g is added, and is warming up to 60 DEG C, and deionized water is added dropwise, and reacts 3 hours, liquid separation
It is that 10%NaOH alkali carries out alkali cyclization 3 hours to take organic phase to add mass concentration, and liquid separation again obtains organic phase, through essence
Thick Jiale muskiness is obtained after evaporating, and handles to have the Jiale muskiness 11.7g of strong muskiness, yield at 50 DEG C with ethyl alcohol recrystallization
91%.
【Embodiment 4】
(1) pentamethyl indane is synthesized
Sulfonic acid type storng-acid cation exchange resin 3.2g prepared by tert-pentyl alcohol 44g and embodiment 1 is added in reactor,
α-methylstyrene 50g is added dropwise into reactor while stirring again；Mixing speed and drop speed are controlled, it is small that 10 are reacted at 30 DEG C
When.For material after reaction through standing, being layered, filtering to isolate sulfonic acid type storng-acid cation exchange resin fat catalyst can be sharp again
With organic phase detaches unreacted raw material through rectifying and obtains indane 64.3g, yield 76%；
(2) hexamethyl indanol is synthesized
Pentamethyl indane 37.6g and 150mL dichloromethane is added in reactor, nothing is added at being -10 DEG C in temperature
Water 0.8g ZnCl2, and turn on agitator, the 20mL dichloromethane that 15.6g propylene oxide is slowly added to after stirring a period of time are molten
Liquid after the reaction was continued 10 hours, is added in mixture of ice and water, is sufficiently stirred, stands, be layered, isolate lower layer's organic phase.It is organic
It is mutually washed in turn with 10%NaOH solution, saturated salt solution and deionized water, is washed till neutrality, is dried to obtain thick indanol.It will be thick
Indanol, which moves into, carries out the faint yellow sticky oily liquids 11g of rectifying, i.e. indanol in flask.
(3) Jiale muskiness is synthesized
Indanol 9.84g and dichloromethane 50mL are added in reactor, phosphorus pentachloride 24.96g is then slowly added into,
Continue stirring 30 minutes, metaformaldehyde 6.6g is added, be warming up to 60 DEG C, deionized water is added dropwise, reacts 3 hours, liquid separation takes organic
It is that 10%NaOH alkali carries out alkali cyclization 3 hours mutually to add mass concentration, and liquid separation again obtains organic phase, after rectifying
To thick Jiale muskiness, handle to have the Jiale muskiness 9.5g of strong muskiness, yield 92% at 50 DEG C with ethyl alcohol recrystallization.
【Comparative example 1】
(1) pentamethyl indane is synthesized
98% sulfuric acid of tert-pentyl alcohol 88g and 20g are added in reactor, then Alpha-Methyl is added dropwise into reactor while stirring
Styrene 100g；Mixing speed and drop speed are controlled, is reacted 10 hours at 40 DEG C.Material after reaction is organic through standing, being layered
Mutually unreacted raw material is detached through rectifying obtain indane 98g, yield 58%.
(2) hexamethyl indanol is synthesized
Pentamethyl indane 18.8g and 100mL dichloromethane is added in reactor, nothing is added at being -15 DEG C in temperature
Water 1.3g ZnCl2, and turn on agitator, the 30mL dichloromethane that 29g propylene oxide is slowly added to after stirring a period of time are molten
Liquid after the reaction was continued 10 hours, is added in mixture of ice and water, is sufficiently stirred, stands, be layered, isolate lower layer's organic phase.It is organic
It is mutually washed in turn with 10%NaOH solution, saturated salt solution and deionized water, is washed till neutrality, is dried to obtain thick indanol.It will be thick
Indanol, which moves into, carries out the faint yellow sticky oily liquids 20g of rectifying, i.e. indanol in flask.
(3) Jiale muskiness is synthesized
Indanol 12.3g and dichloromethane 100mL are added in reactor, phosphorus pentachloride is then slowly added into
24.96g continues stirring 30 minutes, and metaformaldehyde 9.9g is added, and is warming up to 60 DEG C, and deionized water is added dropwise, and reacts 3 hours, liquid separation
It is that 10%NaOH alkali carries out alkali cyclization 3 hours to take organic phase to add mass concentration, and liquid separation again obtains organic phase, through essence
Thick Jiale muskiness is obtained after evaporating, and handles to have the Jiale muskiness 11.7g of strong muskiness, yield at 50 DEG C with ethyl alcohol recrystallization
91%.
【Comparative example 2】
(1) pentamethyl indane is synthesized
98% sulfuric acid of tert-pentyl alcohol 88g and 20g are added in reactor, then Alpha-Methyl is added dropwise into reactor while stirring
Styrene 100g；Mixing speed and drop speed are controlled, is reacted 10 hours at 40 DEG C.Material after reaction is organic through standing, being layered
Mutually unreacted raw material is detached through rectifying obtain indane 98g, yield 58%.
(2) hexamethyl indanol is synthesized
Pentamethyl indane 18.8g and 100mL dichloromethane is added in reactor, nothing is added at being -15 DEG C in temperature
Water 1.3g ZnCl2, and turn on agitator, the 30mL dichloromethane that 25g propylene oxide is slowly added to after stirring a period of time are molten
Liquid after the reaction was continued 10 hours, is added in mixture of ice and water, is sufficiently stirred, stands, be layered, isolate lower layer's organic phase.It is organic
It is mutually washed in turn with 10%NaOH solution, saturated salt solution and deionized water, is washed till neutrality, is dried to obtain thick indanol.It will be thick
Indanol, which moves into, carries out the faint yellow sticky oily liquids 18g of rectifying, i.e. indanol in flask.
(3) Jiale muskiness is synthesized
Indanol 12.3g and dichloromethane 100mL are added in reactor, phosphorus pentachloride is then slowly added into
24.96g continues stirring 30 minutes, and metaformaldehyde 6.6g is added, and is warming up to 60 DEG C, and deionized water is added dropwise, and reacts 3 hours, liquid separation
It is that 10%NaOH alkali carries out alkali cyclization 3 hours to take organic phase to add mass concentration, and liquid separation again obtains organic phase, through essence
Thick Jiale muskiness is obtained after evaporating, and handles to have the Jiale muskiness 11.2g of strong muskiness, yield at 50 DEG C with ethyl alcohol recrystallization
89%.
Above description has fully disclosed the specific implementation mode of the present invention.It should be pointed out that being familiar with the field
Technical staff is to any change for being done of specific implementation mode of the present invention all without departing from the range of claims of the present invention.
Correspondingly, the scope of the claims of the invention is also not limited only to previous embodiment.
Claims (8)
1. a kind of green synthesis process of Jiale muskiness, includes the following steps：
(1) pentamethyl indane is synthesized
Tert-pentyl alcohol and sulfonic acid type storng-acid cation exchange resin are added in reactor, then is dripped while stirring into reactor
Add α-methylstyrene；Mixing speed and drop speed are controlled, is reacted 3~10 hours；Material after reaction is filtered through standing, being layered
It is recycling to isolate sulfonic acid type strong acid cation exchange resin catalyst, organic phase detaches unreacted raw material through rectifying and obtains
To indane；
(2) hexamethyl indanol is synthesized
Pentamethyl indane and organic solvent are added in reactor, anhydrous ZnCl is added at being -15~-10 DEG C in temperature2, and
Turn on agitator is slowly added to propylene oxide solution after stirring a period of time, and after the reaction was continued 5~10 hours, it is mixed that ice water is added
It closes in object, is sufficiently stirred, stands, be layered, isolate lower layer's organic phase；Organic phase 10%NaOH solution, saturated salt solution and
Deionized water is washed in turn, is washed till neutrality, obtains thick indanol；It is faint yellow sticky that thick indanol is moved into progress rectifying in flask
Oily liquids, i.e. indanol；
(3) Jiale muskiness is synthesized
Indanol and organic solvent are added in reactor, phosphorus pentachloride is then slowly added into, continues stirring 20~30 minutes,
Metaformaldehyde is added, is warming up at 50~60 DEG C and deionized water is added dropwise, reacts 3~5 hours, liquid separation takes organic phase to add quality
A concentration of 10%NaOH carries out alkali cyclization 1~3 hour, and liquid separation again obtains organic phase, and thick good happy musk deer is obtained after rectifying
Perfume (or spice) handles to have the Jiale muskiness of strong muskiness at 50 DEG C with ethyl alcohol recrystallization.
2. the green synthesis process of Jiale muskiness according to claim 1, it is characterised in that：In step 1), reacts and be
The temperature of solvent-free reaction, reaction is 30~50 DEG C, and the molar ratio of tert-pentyl alcohol and α-methylstyrene is 1:1~2:1, catalyst
Dosage be tert-pentyl alcohol quality 1~10%.
3. the green synthesis process of Jiale muskiness according to claim 1, it is characterised in that：The sulfonic acid type highly acid sun
The preparation method of ion exchange resin includes the following steps：
(1) by acrylic compounds ethylene oxidic ester, the mixture solution of the mixture of divinylbenzene and initiator and pH be 10~
Suspension polymerization is carried out after the aqueous solution mixing of 12 hydrosol, obtains bead cross-linked copolymer skeleton；
(2) the bead cross-linked copolymer skeleton obtained in step (1), the aqueous solution of sulfamate and sweller are mixed,
The sulfonic acid type storng-acid cation exchange resin is obtained by the reaction under being 8~12 in pH.
4. the green synthesis process of Jiale muskiness according to claim 3, it is characterised in that：The polymerisation temperature
Degree is 75~90 DEG C, and the reaction time is 3~5 hours.
5. the green synthesis process of Jiale muskiness according to claim 3, it is characterised in that：The hydrosol is selected from bright
Glue, hydroxymethyl cellulose, polyvinyl alcohol and combination thereof, dosage is 0.65~0.7% weight of oil phase raw material, water-soluble
0.5%~5% weight of concentration of liquid；The initiator is dibenzoyl peroxide or azodiisobutyronitrile, accounts for oil phase raw material
0.15~0.2% weight.
6. the green synthesis process of Jiale muskiness according to claim 3, it is characterised in that：Wherein the sweller is
The weight ratio of dichloroethanes or N, N- diformazan subunit formamides, bead crosslinked resin skeleton and sweller is 1:2~1:4；And
The sulfamate is sylvite or sodium salt, a concentration of 5~15% weight of the aqueous solution of the sulfamate.
7. the green synthesis process of Jiale muskiness according to claim 1, it is characterised in that：In step 2), You Jirong
Agent is selected from dichloromethane, 1,2- dichloroethanes, chlorobenzene equal solvent, and the molar ratio of pentamethyl indane and propylene oxide is 1:5~
1:10；The dosage of aluminum trichloride (anhydrous) is pentamethyl indane 1~5 (mol) %.
8. the green synthesis process of Jiale muskiness according to claim 1, it is characterised in that：In step 3), You Jirong
Agent is selected from tetrahydrofuran, dichloromethane, 1,2- dichloroethanes etc.；The molar ratio of indanol and phosphorus pentachloride is 1:1.2~1:
1.5；The molar ratio of metaformaldehyde and indanol is 1:1~1:2.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110563692A (en) * | 2019-08-15 | 2019-12-13 | 安徽金禾实业股份有限公司 | Method for preparing galaxolide musk by using superfine aluminum trichloride as catalyst |
| CN111170829A (en) * | 2020-02-28 | 2020-05-19 | 万华化学集团股份有限公司 | Preparation method of hexamethyl indanol |
| CN111848326A (en) * | 2020-07-21 | 2020-10-30 | 安徽金轩科技有限公司 | Industrial treatment method for recycling pentamethyl indane |
| CN112321557A (en) * | 2020-09-14 | 2021-02-05 | 万华化学集团股份有限公司 | Preparation method of Jiale musk |
| CN113185487A (en) * | 2021-04-28 | 2021-07-30 | 安徽金轩科技有限公司 | Production process of Jiale musk |
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