CN107047553A - A kind of efficient mosquito repelling mosquito-repellent incense and preparation method - Google Patents
A kind of efficient mosquito repelling mosquito-repellent incense and preparation method Download PDFInfo
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
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- A—HUMAN NECESSITIES
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- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/20—Combustible or heat-generating compositions
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N31/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic oxygen or sulfur compounds
- A01N31/08—Oxygen or sulfur directly attached to an aromatic ring system
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N31/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic oxygen or sulfur compounds
- A01N31/08—Oxygen or sulfur directly attached to an aromatic ring system
- A01N31/14—Ethers
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N53/00—Biocides, pest repellants or attractants, or plant growth regulators containing cyclopropane carboxylic acids or derivatives thereof
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N57/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds
- A01N57/10—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-oxygen bonds or phosphorus-to-sulfur bonds
- A01N57/12—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-oxygen bonds or phosphorus-to-sulfur bonds containing acyclic or cycloaliphatic radicals
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
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- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
- A01N65/08—Magnoliopsida [dicotyledons]
- A01N65/36—Rutaceae [Rue family], e.g. lime, orange, lemon, corktree or pricklyash
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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Abstract
The invention provides a kind of efficient mosquito repelling mosquito-repellent incense and preparation method, it is made up of following raw material：Limonin, worm phosphorus in heptan, dichloro chrysanthemum acyl chlorides, Thymol, anise alcohol, Chinese honeylocust root-bark extract, pummelo peel extract, calcium carbonate, starch, water, camphorwood dust.The present invention reduces the chemical analysis content harmful to the person while mosquito eradication, mosquito-repelling function is played, and increases the environmentally friendly component content such as plants essential oil, extract, safety and environmental protection.
Description
Technical field
The present invention relates to a kind of efficient mosquito repelling mosquito-repellent incense and preparation method, belong to mosquito repellent field.
Background technology
Mosquito-repellent incense is a kind of mosquito repellent thing, and the cigarette that medicine therein is ignited being sent afterwards can mosquitoes or smoked dead mosquito.I
State, which kindles mosquito repellent incense, very long history, two kinds of traditional mosquito-repellent incense separated time perfume and incense coil.Containing many in the cigarette of conventional mosquito coil burning
Aromatic hydrocarbon ring (PAHs), carbonyls（Such as formaldehyde and acetaldehyde）With benzene etc., there is certain injury to human body.
The content of the invention
To overcome above-mentioned technical problem, the invention reside in a kind of efficient mosquito repelling mosquito-repellent incense and preparation method is improved, gone out playing
While mosquito, mosquito-repelling function, the chemical analysis content harmful to the person is reduced, increases the environmentally friendly composition such as plants essential oil, extract
Content.
A kind of efficient mosquito repelling mosquito-repellent incense, is prepared from by following percentage by weight raw material：
Limonin 2.2-2.6%, worm phosphorus 0.1-0.2% in heptan, dichloro chrysanthemum acyl chlorides 0.1-0.2%, Thymol 3.6-3.9%, fennel
Alcohol 2-3%, Chinese honeylocust root-bark extract 4.6-5.5%, pummelo peel extract 9-13%, calcium carbonate 8-10%, starch 17-18%, water 8-12%,
Surplus is camphorwood dust.
Further, it is prepared from by following percentage by weight raw material：
Limonin 2.5%, worm phosphorus in heptan 0.12%, dichloro chrysanthemum acyl chlorides 0.13%, Thymol 3.7%, anise alcohol 2.4%, Chinese honeylocust root-bark
Extract 5.1%, pummelo peel extract 10.5%, calcium carbonate 9%, starch 17.4%, water 11%, camphorwood dust 38.15%.
Further, described worm phosphorus in heptan, dichloro chrysanthemum acyl chlorides mass ratio are 1：1.1-1.2.
Further, described Chinese honeylocust root-bark extract, pummelo peel extract mass ratio are 0.1：0.2-0.25.
A kind of preparation method of efficient mosquito repelling mosquito-repellent incense, by limonin, worm phosphorus in heptan, dichloro chrysanthemum acyl chlorides, Thymol, fennel
Starch, water, which are added, after alcohol, Chinese honeylocust root-bark extract, pummelo peel extract, camphorwood dust, calcium carbonate crushing, grinding is mixed into mud
Shape, be then added to it is compressing in mosquito-repellent incense machine, take out drying after, produce.
Further, the synthetic method of described limonin comprises the following steps,
The first step, chromium trioxide is slowly added into acetic anhydride, and question response is stirred to orange, adds raw material obacunone, and rise
Temperature continues to stir 3 hours to 60 DEG C, and the completely rear reaction solution concentration of question response, concentrate extraction is dried, obtains intermediate 2；
Second step；Sodium borohydride in the solvent of intermediate 2, will be slowly added to, not higher than 20 DEG C of temperature in reaction is kept, finishes, react
Continue stirring reaction at 0 DEG C, reaction solution concentration, concentrate washing, organic phase is dried, and concentration is purified by Flash silica post
Obtain intermediate 3；
3rd step, intermediate 3 is dissolved in solvent, adds lithium hydroxide, and reaction is stirred at room temperature, and is extracted, and organic phase is dried,
Filtering, is concentrated to give crude intermediate 4；
4th step, intermediate 4 is dissolved in anhydrous tetrahydro furan, under nitrogen protection, sequentially adds diethyl azodiformate,
Saturated common salt water washing is used in triphenylphosphine, reaction stirring reaction under room temperature under nitrogen protection, reaction after terminating, organic phase is dried,
Concentration, gained residue obtains intermediate 5 by the purifying of Flash silica post；
5th step, intermediate 5 is dissolved in anhydrous tetrahydro furan, and borine tetrahydrofuran solution is slowly added dropwise, and is reacted in room temperature nitrogen
After being stirred 16 hours under gas shielded, H2O2, saturated sodium bicarbonate solution are added to reaction solution, reaction continues to stir 2 at room temperature
Hour, reaction liquid layer, aqueous phase is extracted by ethyl acetate, merges and drying is used after organic phase, and filtering and concentrating, gained residue leads to
Cross quick silicagel column purifying and obtain product intermediate 6；
6th step, intermediate 6 is dissolved in anhydrous tetrahydro furan, under nitrogen protection, sequentially adds diethyl azodiformate,
Triphenylphosphine reaction is stirred 16 hours under room temperature under nitrogen protection, and saturated common salt water washing is used in reaction after terminating, and organic phase is dried,
Filtering and concentrating, gained residue obtains final products limonin by ethyl alcohol recrystallization.
Limonin, worm phosphorus in heptan, dichloro chrysanthemum acyl chlorides, Thymol, anise alcohol, Chinese honeylocust root-bark extract, pummelo peel extract,
Calcium carbonate, starch, water, camphorwood dust.
The present invention is except based on limonin, collocation worm phosphorus in heptan, dichloro chrysanthemum acyl chlorides are strict to control in the efficacy component of mosquito agent
Heptan worm phosphorus, dichloro chrysanthemum acyl chlorides, effectively reduce chemical noxious composition, based on the limonin of safety and environmental protection, can effectively remove mosquito
Son.Thymol, the cooperation of anise alcohol can play increase activity, and the cooperation with worm phosphorus in heptan, dichloro chrysanthemum acyl chlorides is primarily served
The effect of mosquito repellent, and Thymol, anise alcohol are extracted form natural plant, safety and environmental protection.We have found that being extracted by Chinese honeylocust root-bark
The rational proportion of thing, pummelo peel extract, its repelling effect is also very notable.Starch plays a part of bonding, and camphorwood dust is on the one hand
Play a part of burning, meanwhile, cigarette when it burns also has certain repelling effect.
Embodiment
The preparation of the limonin of embodiment 1
Chromium trioxide (11 g, 110 mmol) is slowly added to acetic anhydride (100 mL), question response is stirred to orange at 0 DEG C, plus
Enter raw material obacunone (Obacunone) (45 g, 99.1 mmol), and be warming up to 60 DEG C to continue to stir 3 hours, TLC (PE：
EA=2：1) reaction end is monitored, the completely rear reaction solution concentration of question response, concentrate passes through ethyl acetate (200 mL) and water
(200mL) is layered, and organic phase is dried with magnesium sulfate and concentrated, and intermediate 2 (46.0 g, 98.2 mmol) is dissolved in into tetrahydrofuran
In (200 mL) and methanol (20 mL), sodium borohydride (6.0 g, 150 mmol) is slowly added at 0 DEG C, the interior temperature of reaction is kept not
Higher than 20 DEG C, finish, reaction continues to stir 1 hour at 0 DEG C, TLC (PE:EA=1:1) display reaction terminates, and reaction solution is dense
Contracting, concentrate ethyl acetate (200 mL) dissolves, successively with saturated sodium bicarbonate (100 mL), water (100 mL), and saturation
Saline solution (100 mL) is washed, and organic phase is concentrated with magnesium sulfate dry filter, and remaining crude product is obtained by the purifying of Flash silica post
The product of intermediate 3 (33.0 g, yield 70%), eluant, eluent is petroleum ether (PE):Ethyl acetate (EA)=1:1；By intermediate 3
(33.0 g, 70.2 mmol) are dissolved in the mixed solution of tetrahydrofuran (100 mL) and methanol (100 mL), add hydroxide
Lithium (2.4 g, 100 mmol), reaction is stirred at room temperature 3 hours, TLC (PE:EA=1:1) display reaction raw materials disappear, reaction
Product adjusts pH=5~6, and ethyl acetate (2 × 100 mL) extraction merges organic phase and dried with magnesium sulfate, filters, be concentrated to give
Crude intermediate 4 (24.0 g, yield 71%)；Intermediate 4 (24.0 g, 49.2 mmol) is dissolved in anhydrous tetrahydro furan
In (300 mL), under nitrogen protection, diethyl azodiformate (DEAD) (10.5 g, 60.0 mmol), triphen are sequentially added
Base phosphine (15.7 g, 60.0 mmol), reaction is stirred 16 hours under room temperature under nitrogen protection, TLC (PE:EA=1:1) monitoring reaction
Terminate, reaction is washed after terminating with saturated aqueous common salt (3 × 50 mL), organic phase is concentrated with magnesium sulfate dry filter, gained is remaining
Thing obtains intermediate 5 by the purifying of Flash silica post, and (18.0 g, yield is that 78%), eluant, eluent is petroleum ether (PE):Acetic acid second
Ester (EA)=2:1；Intermediate 5 (18.0 g, 38.3 mmol) is dissolved in anhydrous tetrahydro furan (200 mL), boron is slowly added dropwise
Alkane tetrahydrofuran solution (50 mL, 1M in THF, 50 mmol), after reaction is stirred 16 hours under room temperature under nitrogen protection, to
Reaction solution adds H2O2 (50 mL), saturated sodium bicarbonate solution (50 mL), and reaction continues to stir 2 hours at room temperature, reaction
Liquid is layered, and aqueous phase is extracted by ethyl acetate (3 × 50 mL), is dried after merging organic phase with magnesium sulfate, filtering and concentrating.Gained
Residue by Flash silica post purifying obtain product intermediate 6 (11.0 g, yield be 58%), eluant, eluent is petroleum ether
(PE):Ethyl acetate (EA)=4:1；Intermediate 6 (11.0 g, 22.5 mmol) is dissolved in anhydrous tetrahydro furan (300 mL)
In, under nitrogen protection, sequentially add diethyl azodiformate (DEAD) (5.9 g, 33.8 mmol), triphenylphosphine (8.9
G, 33.8 mmol), reaction is stirred 16 hours under room temperature under nitrogen protection, TLC (PE:EA=1:1) monitoring reaction terminates, and reacts
Washed after end with saturated aqueous common salt (3 × 50 mL), organic phase is concentrated with magnesium sulfate dry filter, gained residue passes through second
Alcohol is recrystallized to give final products limonin (8.0 g, yield 76%).
Course of reaction is as follows：
Intermediate 5 1H-NMR (400 MHz, MeOD) δ 7.20 (s, 1H), 7.13 (s, 1H), 6.20- 6.05 (m,
3H) 5.39(s,1H), 4.33-4.16(m,2H), 3.21(s,1H), 2.40-2.31(m,2H), 1.81-1.43(m,
6H), 1.30(s, 6H), 1.21(s, 3H),0.93(s, 3H)。
Product limonin 1H-NMR (400 MHz, MeOD) δ 7.23 (s, 1H), 7.11 (s, 1H), 6.13 (s,
1H) 5.52(s,1H), 4.28-4.18(m,3H), 3.35(s,1H), 2.48-2.26(m,5H), 1.62-1.40(m,
5H), 1.26(s, 9H), 0.98(s, 3H); ES-LCMS m/z 471.2 (M+H)。
Embodiment 1
By limonin 2.5g, worm phosphorus 0.12g in heptan, dichloro chrysanthemum acyl chlorides 0.13g, Thymol 3.7g, anise alcohol 2.4g, Chinese honey locust root
Starch 17.4g, water are added after bark extract 5.1g, pummelo peel extract 10.5g, calcium carbonate 9g, camphorwood dust 38.15g crushing, grinding
11g is mixed into pureed, be then added to it is compressing in mosquito-repellent incense machine, take out drying after, produce.
Embodiment 2
By limonin 2.3g, worm phosphorus 0.16g in heptan, dichloro chrysanthemum acyl chlorides 0.14g, Thymol 3.8g, anise alcohol 2.8g, Chinese honey locust root
Starch 18g, water 10g are added after bark extract 4.9g, pummelo peel extract 12g, camphorwood dust 37.5g, calcium carbonate 8.4g crushing, grinding
Be mixed into pureed, be then added to it is compressing in mosquito-repellent incense machine, take out drying after, produce.
Comparative example 1
By worm phosphorus 0.12g in heptan, dichloro chrysanthemum acyl chlorides 0.13g, Thymol 3.7g, anise alcohol 2.4g, Chinese honeylocust root-bark extract 5.1g,
Starch 17.4g, water 11g are added after pummelo peel extract 10.5g, calcium carbonate 9g, camphorwood dust 38.15g crushing, grinding to be mixed into
Pureed, be then added to it is compressing in mosquito-repellent incense machine, take out drying after, produce.
Comparative example 2
By limonin 2.5g, Thymol 3.7g, anise alcohol 2.4g, Chinese honeylocust root-bark extract 5.1g, pummelo peel extract
Starch 17.4g, water 11g are added after 10.5g, calcium carbonate 9g, camphorwood dust 38.15g crushing, grinding and is mixed into pureed, then
Be added to it is compressing in mosquito-repellent incense machine, take out drying after, produce.
Comparative example 3
By limonin 2.5g, worm phosphorus 0.12g in heptan, dichloro chrysanthemum acyl chlorides 0.13g, Chinese honeylocust root-bark extract 5.1g, pummelo peel extract
Starch 17.4g, water 11g are added after 10.5g, calcium carbonate 9g, camphorwood dust 38.15g crushing, grinding and is mixed into pureed, then
Be added to it is compressing in mosquito-repellent incense machine, take out drying after, produce.
Comparative example 4
By limonin 2.5g, worm phosphorus 0.12g in heptan, dichloro chrysanthemum acyl chlorides 0.13g, Thymol 3.7g, anise alcohol 2.4g, calcium carbonate
Starch 17.4g, water 11g are added after 9g, camphorwood dust 38.15g crushing, grinding and is mixed into pureed, are then added to mosquito-repellent incense machine
In it is compressing, take out drying after, produce.
Test：Indoor harmacological effect.Using mosquito-repellent incense indoor harmacological effect assay method and evaluation as defined in the .4-2009 of GB/T 13917
Standard is tested.Test object is the mosquito-repellent incense obtained by embodiment 1-2, comparative example 1-4.
The evaluation index of the testing result is as follows：Pharmacodynamic results are divided into A, B two-stage, do not reach B grades of standard persons and belong to and do not conform to
Lattice product.Wherein, A grades：KT50≤4 .0 minutes；B grades≤8.0 minutes.
Test result is as follows：
| KT50(sec) | |
| Embodiment 1 | 96 |
| Embodiment 2 | 101 |
| Comparative example 1 | 152 |
| Comparative example 2 | 159 |
| Comparative example 3 | 131 |
| Comparative example 4 | 138 |
From above-described embodiment, it can be seen that when in composition of the present invention contain limonin, worm phosphorus in heptan, dichloro chrysanthemum acyl chlorides, hundred in
When fragrant phenol, anise alcohol, Chinese honeylocust root-bark extract, pummelo peel extract, its repelling effect is optimal, and has lacked limonin, or worm in heptan
When phosphorus, dichloro chrysanthemum acyl chlorides, or in fragrant phenol, anise alcohol when, or when Chinese honeylocust root-bark extract, pummelo peel extract, its repelling effect is equal
Difference.
Although the embodiment to the present invention gives detailed description and illustrated above, it should be noted that
We can carry out various equivalent changes and modification according to the conception of the present invention to above-mentioned embodiment, and the function produced by it is made
, all should be within protection scope of the present invention during with the spirit still covered without departing from specification.
Claims (6)
1. a kind of efficient mosquito repelling mosquito-repellent incense, it is characterised in that be prepared from by following percentage by weight raw material：
Limonin 2.2-2.6%, worm phosphorus 0.1-0.2% in heptan, dichloro chrysanthemum acyl chlorides 0.1-0.2%, Thymol 3.6-3.9%, fennel
Alcohol 2-3%, Chinese honeylocust root-bark extract 4.6-5.5%, pummelo peel extract 9-13%, calcium carbonate 8-10%, starch 17-18%, water 8-12%,
Surplus is camphorwood dust.
2. a kind of efficient mosquito repelling mosquito-repellent incense according to claim 1, it is characterised in that prepared by following percentage by weight raw material
Form：
Limonin 2.5%, worm phosphorus in heptan 0.12%, dichloro chrysanthemum acyl chlorides 0.13%, Thymol 3.7%, anise alcohol 2.4%, Chinese honeylocust root-bark
Extract 5.1%, pummelo peel extract 10.5%, calcium carbonate 9%, starch 17.4%, water 11%, camphorwood dust 38.15%.
3. a kind of efficient mosquito repelling mosquito-repellent incense according to claim 1, it is characterised in that described worm phosphorus in heptan, dichloro chrysanthemum acyl chlorides
Mass ratio is 1：1.1-1.2.
4. a kind of efficient mosquito repelling mosquito-repellent incense according to claim 1, it is characterised in that described Chinese honeylocust root-bark extract, shaddock
Bark extract mass ratio is 0.1：0.2-0.25.
5. according to a kind of preparation method of any described efficient mosquito repelling mosquito-repellent incenses of claim 1-4, it is characterised in that lemon is bitter
Element, worm phosphorus in heptan, dichloro chrysanthemum acyl chlorides, Thymol, anise alcohol, Chinese honeylocust root-bark extract, pummelo peel extract, camphorwood dust, calcium carbonate
Crush, add starch, water after grinding and be mixed into pureed, be then added to compressing in mosquito-repellent incense machine, take out after drying, i.e.,
.
6. a kind of preparation method of efficient mosquito repelling mosquito-repellent incense according to claim 5, it is characterised in that described limonin
Synthetic method comprise the following steps,
The first step, chromium trioxide is slowly added into acetic anhydride, and question response is stirred to orange, adds raw material obacunone, and rise
Temperature continues to stir 3 hours to 60 DEG C, and the completely rear reaction solution concentration of question response, concentrate extraction is dried, obtains intermediate 2；
Second step；Sodium borohydride in the solvent of intermediate 2, will be slowly added to, not higher than 20 DEG C of temperature in reaction is kept, finishes, react
Continue stirring reaction at 0 DEG C, reaction solution concentration, concentrate washing, organic phase is dried, and concentration is purified by Flash silica post
Obtain intermediate 3；
3rd step, intermediate 3 is dissolved in solvent, adds lithium hydroxide, and reaction is stirred at room temperature, and is extracted, and organic phase is dried,
Filtering, is concentrated to give crude intermediate 4；
4th step, intermediate 4 is dissolved in anhydrous tetrahydro furan, under nitrogen protection, sequentially adds diethyl azodiformate,
Saturated common salt water washing is used in triphenylphosphine, reaction stirring reaction under room temperature under nitrogen protection, reaction after terminating, organic phase is dried,
Concentration, gained residue obtains intermediate 5 by the purifying of Flash silica post；
5th step, intermediate 5 is dissolved in anhydrous tetrahydro furan, and borine tetrahydrofuran solution is slowly added dropwise, and is reacted in room temperature nitrogen
After being stirred 16 hours under gas shielded, H2O2, saturated sodium bicarbonate solution are added to reaction solution, reaction continues to stir 2 at room temperature
Hour, reaction liquid layer, aqueous phase is extracted by ethyl acetate, merges and drying is used after organic phase, and filtering and concentrating, gained residue leads to
Cross quick silicagel column purifying and obtain product intermediate 6；
6th step, intermediate 6 is dissolved in anhydrous tetrahydro furan, under nitrogen protection, sequentially adds diethyl azodiformate,
Triphenylphosphine reaction is stirred 16 hours under room temperature under nitrogen protection, and saturated common salt water washing is used in reaction after terminating, and organic phase is dried,
Filtering and concentrating, gained residue obtains final products limonin by ethyl alcohol recrystallization.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710231369.7A CN107047553A (en) | 2017-04-11 | 2017-04-11 | A kind of efficient mosquito repelling mosquito-repellent incense and preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710231369.7A CN107047553A (en) | 2017-04-11 | 2017-04-11 | A kind of efficient mosquito repelling mosquito-repellent incense and preparation method |
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| CN106172389A (en) * | 2016-07-15 | 2016-12-07 | 抚州泰菊实业有限公司 | A kind of natural plants mosquito incense and preparation method thereof |
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| CN106172389A (en) * | 2016-07-15 | 2016-12-07 | 抚州泰菊实业有限公司 | A kind of natural plants mosquito incense and preparation method thereof |
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| G. K. JAYAPRAKASHA ET AL: ""Limonoids from Citrus reticulata and their moult inhibiting activity in mosquito Culex quinquefasciatus larvae"", 《 PHYTOCHEMISTRY》 * |
| 杨晓伟: ""植物源蚊香增效剂的研究与开发"", 《中国优秀硕士学位论文全文数据库工程科技I辑》 * |
| 林青: "《"21世纪十万个为什么-植物奇观"》", 31 January 2010, 北京工业大学出版社 * |
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