Preparation method of galaxolide

Abstract

The present invention relates to a preparation method of galaxolide, comprising: preparing herb alcohol into herb alcoholate; reacting the herb alcoholate with a compound having a structural formula as shown in formula (1) to generate an intermediate having a structural formula as shown in formula (2), wherein in formula (1), R is a halogen element; and subjecting the intermediate to a transesterification reaction with methyl propionate under the action of a transesterification catalyst to obtain galaxolide. In the preparation method of galaxolide of the present invention, the raw materials and reactants are widely sourced, low in price, low in production cost, and the yield of galaxolide is high.

Description

Technical Field

[0001] The present invention relates to the technical field of spices, and particularly to a preparation method of Hivone musk. Background Art

[0002] Hivone musk is a musk with very delicate aroma. It is a musk aroma with complex aroma and modern texture, accompanied by the aroma of pear fruit. The aroma of Hivone musk is between δ-decalactone and musk T, and can be used for perfume blending in perfumes, toiletries and daily necessities.

[0003] The traditional production process of Hivone musk is obtained by the addition reaction of herb alcohol and isobutene oxide, and then the esterification reaction with propionic anhydride. However, the raw materials isobutene oxide and propionic anhydride used in this synthesis method are expensive, which increases the production cost, and the yields of herb alcohol and isobutene oxide are low, which is not conducive to industrial production. Summary of the Invention

[0004] Based on this, in view of the above problems, it is necessary to provide a preparation method of Hivone musk. The raw materials and reactants of this preparation method are widely sourced, inexpensive, have low production costs, and have a high yield of Hivone musk.

[0005] A preparation method of Hivone musk includes the following steps:

[0006] Preparing herb alcoholate from herb alcohol;

[0007] Reacting the herb alcoholate with a compound having the structure shown in formula (1) to form an intermediate having the structure shown in formula (2);

[0008] Performing a transesterification reaction on the intermediate and methyl propionate under the action of a transesterification catalyst to obtain Hivone musk;

[0009]

[0010] In formula (1), R is a halogen element.

[0011] In one embodiment, the step of preparing herb alcoholate from herb alcohol includes: reacting herb alcohol with a strong base to obtain herb alcoholate.

[0012] In one embodiment, the strong base is selected from at least one of potassium hydroxide and sodium hydroxide.

[0013] In one embodiment, the molar ratio of the herb alcohol to the strong base is 1:1 - 1:5.

[0014] In one embodiment, in the step of reacting the herb alcohol with the strong base, the reaction temperature is 120°C - 180°C.

[0015] In one embodiment, the compound represented by the structural formula as shown in formula (1) is selected from 2-fluoro-2-methyl-1-propanol.

[0016] In one embodiment, the molar ratio of the herb alcoholate to the compound represented by the structural formula as shown in formula (1) is 1:1 - 1:3.

[0017] In one embodiment, in the step of reacting the herb alcoholate with the compound represented by the structural formula as shown in formula (1), the reaction temperature is 80°C - 120°C.

[0018] In one embodiment, the molar ratio of the intermediate to the methyl propionate is 1:1 - 1:5.

[0019] In one embodiment, in the step of transesterifying the intermediate and methyl propionate under the action of a transesterification catalyst, the reaction temperature is 100°C - 190°C.

[0020] In the method for preparing civetone of the present invention, using herb alcohol as a raw material, civetone is produced through three-step reactions. Among them, the raw materials and reactants are widely sourced and inexpensive. Meanwhile, no catalyst is required during the reaction process of converting herb alcohol to herb alcoholate and during the reaction of herb alcoholate with the compound represented by formula (2). Moreover, the catalyst for the transesterification reaction can be recycled and reused, and no solvent is needed in the three-step reactions, further reducing the production cost of civetone. Additionally, due to the good selectivity and high conversion rate during the reaction process, the generation of by-products is reduced, resulting in high yields of the intermediate and civetone and low production costs. Detailed Embodiments

[0021] To facilitate the understanding of the present invention, the present invention will be described more comprehensively below with reference to relevant embodiments. However, the present invention can be implemented in many different forms and is not limited to the embodiments described herein. On the contrary, these embodiments are provided to make the understanding of the disclosure of the present invention more thorough and comprehensive.

[0022] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by those of ordinary skill in the technical field to which the present invention belongs. The terms used in the specification of the present invention herein are only for the purpose of describing specific embodiments and are not intended to limit the present invention. The term "and / or" used herein includes any and all combinations of one or more of the related listed items.

[0023] The method for preparing civetone provided by the present invention includes the following steps:

[0024] S11, preparing herb alcoholate from herb alcohol.

[0025] In step S11, the source of herb alcohol is not limited. Commercially available herb alcohol can be directly purchased, or it can be obtained by hydrolyzing avermectin ester under alkaline conditions. In one embodiment, the preparation steps of herb alcohol are specifically as follows: Add water, sodium hydroxide, ethanol, and avermectin ester to a reaction vessel. After mixing, heat to 90°C - 100°C and react for 2h - 4h to obtain a reaction solution. Then, add a 5% formic acid aqueous solution to the reaction solution for extraction, remove the aqueous phase, add a 6% sodium bicarbonate aqueous solution to the organic phase for continuous extraction, remove the aqueous phase, and finally dry the organic phase to obtain herb alcohol.

[0026] There are various ways to prepare herb alcohol salt. Herb alcohol can be reacted with an active metal to form herb alcohol salt, or it can be reacted with a strong base to form herb alcohol salt. In the present invention, it is preferably to react herb alcohol with a strong base to form herb alcohol salt.

[0027] In one embodiment, in the step of reacting herb alcohol with a strong base, the strong base is selected from at least one of potassium hydroxide and sodium hydroxide. When the strong base is potassium hydroxide, the obtained herb alcohol salt is potassium herb alcoholate; when the strong base is sodium hydroxide, the obtained herb alcohol salt is sodium herb alcoholate.

[0028] Taking sodium hydroxide as an example, the reaction formula of herb alcohol and sodium hydroxide is:

[0029]

[0030] The reaction of herb alcohol with a strong base to form herb alcohol salt needs to be carried out under high-temperature dehydration. In addition to forming herb alcohol salt during the reaction, water is also generated. The formed herb alcohol salt will be decomposed into herb alcohol and a strong base in the presence of water. Therefore, the reaction temperature in this reaction is higher than the boiling point of water, so that the water generated during the reaction will be directly distilled out of the reaction system, achieving the effect of dehydration, enabling herb alcohol to continue to react with the strong base to form herb alcohol salt, and the formed herb alcohol salt will not be decomposed into herb alcohol and a strong base, improving the stability and yield of herb alcohol salt. In addition, the reaction of herb alcohol with a strong base does not require the participation of a solvent and a catalyst, reducing the production cost.

[0031] In order to better improve the reaction rate, reduce the occurrence of side reactions, and better remove by-products during the reaction, in one embodiment, in the step of reacting herb alcohol with a strong base, the reaction temperature is 120°C - 180°C, preferably 110°C - 150°C.

[0032] In order to better form herb alcohol salt, in one embodiment, the molar ratio of herb alcohol to the strong base is 1:1 - 1:5, preferably 1:1.2 - 1:2.

[0033] S12. React the herb alcoholate with the compound having the structural formula shown in Formula (1) to form an intermediate having the structural formula shown in Formula (2).

[0034]

[0035] In Formula (1), R is a halogen element, and the halogen element is selected from chlorine, bromine, iodine, etc. Further, the compound having the structural formula shown in Formula (1) is preferably 2-fluoro-2-methyl-1-propanol.

[0036] Taking 2-fluoro-2-methyl-1-propanol as an example, the reaction formula of the herb alcoholate and 2-fluoro-2-methyl-1-propanol is:

[0037]

[0038] In step S12, since the generated intermediate having the structural formula shown in Formula (2) is immiscible with the residual herb alcoholate after the reaction and the intermediate is insoluble in water, the residual herb alcoholate after the reaction can be removed by washing with water after the reaction, and then the intermediate can be obtained by vacuum distillation, and the operation is simple. At the same time, the compound having the structural formula shown in Formula (1) is inexpensive, and no solvent and catalyst are required in the whole reaction process, further reducing the production cost.

[0039] In order to better generate the intermediate having the structural formula shown in Formula (2), in one embodiment, the molar ratio of the herb alcoholate to the compound having the structural formula shown in Formula (1) is 1:1 - 1:3, preferably 1:1.2 - 1:2.

[0040] In order to better improve the reaction rate and reduce the generation of side reactions, in one embodiment, in the step of reacting the herb alcoholate with the compound having the structural formula shown in Formula (1), the reaction temperature is 80°C - 120°C, preferably 100°C - 110°C.

[0041] S13. Perform a transesterification reaction on the intermediate and methyl propionate under the action of a transesterification catalyst to obtain galaxolide, and the reaction formula is as follows:

[0042]

[0043] Among them, the transesterification catalyst can be selected from common acidic catalysts or basic catalysts. In one embodiment, the transesterification catalyst is selected from at least one of sodium carbonate, potassium carbonate, sodium methoxide methanol solution, p-toluenesulfonic acid, di-n-butyltin oxide, and isopropyl titanate, and preferably di-n-butyltin oxide.

[0044] During the transesterification reaction, in addition to generating intermediates, methanol is also produced. However, since the boiling point of methanol is lower than the reaction temperature of the transesterification reaction, it will be directly distilled out of the reaction system during the reaction. Since the transesterification reaction is a reversible reaction, the distillation of methanol will cause the reaction to shift in the direction of generating intermediates, thereby increasing the reaction rate and improving the yield of intermediates. In addition, solvents are not required during the transesterification reaction, and the transesterification catalyst in the reaction can be recycled, so the production cost can be reduced.

[0045] In order to better increase the reaction rate, reduce the generation of side reactions, and better remove by-products during the reaction, in one embodiment, in the step of carrying out the transesterification reaction of the intermediate and methyl propionate under the action of a transesterification catalyst, the reaction temperature is 100°C - 190°C, preferably 130°C - 150°C.

[0046] In order to better generate civetone musk, in one embodiment, the molar ratio of the intermediate to the methyl propionate is 1:1 - 1:5, preferably 1:1.2 - 1:2.

[0047] It should be noted that the civetone musk crude product is obtained after carrying out the transesterification reaction of the intermediate and methyl propionate under the action of a transesterification catalyst, and the civetone musk crude product is obtained through methods such as vacuum distillation to obtain civetone musk.

[0048] In the preparation method of civetone musk of the present invention, using herb alcohol as a raw material, civetone musk is generated through three steps of reactions. Among them, the raw materials and reactants are widely sourced and inexpensive. At the same time, no catalyst is required during the reaction of herb alcohol to generate herb alcoholate and during the reaction of herb alcoholate with the compound shown in formula (2). The transesterification catalyst can be recycled, and no solvent is required in the three-step reaction, further reducing the production cost of civetone musk. In addition, due to the good selectivity and high conversion rate during the reaction process, the generation of by-products is reduced, resulting in high yields of intermediates and civetone musk and low production costs.

[0049] Hereinafter, the preparation method of the civetone musk will be further described through the following specific examples.

[0050] Example 1

[0051] 312 g of herb alcohol and 120 g of sodium hydroxide were put into a 1000 mL three-necked flask and reacted at a temperature of 130°C. The water generated during the reaction was distilled out, and it was in a full-discharge state. Samples were taken during the reaction for gas chromatography analysis. When the mass content of herb alcohol ≤ 0.5%, the reaction was stopped, and 321.54 g of herb alcoholate with a content of 92.87% was obtained after washing with water.

[0052] 178 g of the sodium herbate obtained above and 138 g of 2-fluoro-2-methyl-1-propanol were put into a 1000 mL three-necked flask and reacted at a temperature of 80 °C. Samples were taken during the reaction for gas chromatography analysis. When the mass content of 2-fluoro-2-methyl-1-propanol ≤ 0.5%, the reaction was stopped. The sodium herbate was removed by washing with water to obtain a crude product with a content of 87.32%. Then, it was distilled under reduced pressure to obtain 165.14 g of an intermediate with a content of 96.76%.

[0053] 114 g of the intermediate obtained above, 66 g of methyl propionate and 5 g of dibutyltin oxide were put into a 1000 mL three-necked flask and reacted at a temperature of 150 °C. Samples were taken during the reaction for gas chromatography analysis. When the mass content of the intermediate ≤ 0.5%, the reaction was stopped to obtain a crude product with a content of 93.17%. It was rectified under reduced pressure to obtain 118.48 g of galaxolide with a content of 97.63%.

[0054] Example 2

[0055] 312 g of herb alcohol and 80 g of sodium hydroxide were put into a 1000 mL three-necked flask and reacted at a temperature of 120 °C. The water generated during the reaction was distilled out to be in a full discharge state. Samples were taken during the reaction for gas chromatography analysis. When the mass content of herb alcohol ≤ 0.5%, the reaction was stopped. After washing with water, 296.16 g of sodium herbate with a content of 72.11% was obtained.

[0056] 178 g of the sodium herbate obtained above and 92 g of 2-fluoro-2-methyl-1-propanol were put into a 1000 mL three-necked flask and reacted at a temperature of 80 °C. Samples were taken during the reaction for gas chromatography analysis. When the mass content of 2-fluoro-2-methyl-1-propanol ≤ 0.5%, the reaction was stopped to obtain a crude product with a content of 49.45%. The sodium herbate was removed by washing with water, and then it was distilled under reduced pressure to obtain 102.52 g of an intermediate with a content of 96.27%.

[0057] 102.50 g of the intermediate obtained above, 40.00 g of methyl propionate and 5 g of dibutyltin oxide were put into a 1000 mL three-necked flask and reacted at a temperature of 150 °C. Samples were taken during the reaction for gas chromatography analysis. When the mass content of the intermediate ≤ 0.5%, the reaction was stopped to obtain a crude product with a content of 88.15%. It was rectified under reduced pressure to obtain 105.99 g of galaxolide with a content of 97.15%.

[0058] Example 3

[0059] 312 g of herb alcohol and 400 g of sodium hydroxide were put into a 1000 mL three-necked flask, and the reaction was carried out at a temperature of 150 °C. The water generated during the reaction was distilled out, and it was in a full-discharge state. Samples were taken during the reaction for gas chromatography analysis. When the mass content of herb alcohol ≤ 0.5%, the reaction was stopped, and after washing with water, 304.85 g of sodium herb alcohol with a content of 82.46% was obtained.

[0060] 178 g of the sodium herb alcohol obtained above and 276 g of 2-fluoro-2-methyl-1-propanol were put into a 1000 mL three-necked flask, and the reaction was carried out at a temperature of 80 °C. Samples were taken during the reaction for gas chromatography analysis. When the mass content of 2-fluoro-2-methyl-1-propanol ≤ 0.5%, the reaction was stopped, and a crude product with a content of 77.58% was obtained. After washing with water to remove sodium herb alcohol, it was then distilled under reduced pressure to obtain 159.42 g of an intermediate with a content of 95.83%.

[0061] 114 g of the intermediate obtained above, 220 g of methyl propionate and 5 g of dibutyltin oxide were put into a 1000 mL three-necked flask, and the reaction was carried out at a temperature of 150 °C. Samples were taken during the reaction for gas chromatography analysis. When the mass content of the intermediate ≤ 0.5%, the reaction was stopped, and the crude product had a content of 89.14%. After vacuum rectification, 113.92 g of galaxolide with a content of 97.26% was obtained.

[0062] Example 4

[0063] 312 g of herb alcohol and 96 g of sodium hydroxide were put into a 1000 mL three-necked flask, and the reaction was carried out at a temperature of 120 °C. The water generated during the reaction was distilled out, and it was in a full-discharge state. Samples were taken during the reaction for gas chromatography analysis. When the mass content of herb alcohol ≤ 0.5%, the reaction was stopped, and after washing with water, 308.59 g of sodium herb alcohol with a content of 94.28% was obtained.

[0064] 178 g of the sodium herb alcohol obtained above and 110 g of 2-fluoro-2-methyl-1-propanol were put into a 1000 mL three-necked flask, and the reaction was carried out at a temperature of 80 °C. Samples were taken during the reaction for gas chromatography analysis. When the mass content of 2-fluoro-2-methyl-1-propanol ≤ 0.5%, the reaction was stopped, and a crude product with a content of 90.11% was obtained. After washing with water to remove sodium herb alcohol, it was then distilled under reduced pressure to obtain 180.07 g of an intermediate with a content of 96.89%.

[0065] 114 g of the intermediate obtained above, 52.80 g of methyl propionate and 5 g of dibutyltin oxide were put into a 1000 mL three-necked flask and reacted at a temperature of 150 °C. Samples were taken during the reaction for gas chromatography analysis. When the mass content of the intermediate ≤ 0.5%, the reaction was stopped, and a crude product with a content of 94.13% was obtained. Vacuum distillation gave 118.95 g of galaxolide with a content of 97.89%.

[0066] Example 5

[0067] 312 g of herb alcohol and 160 g of sodium hydroxide were put into a 1000 mL three-necked flask and reacted at a temperature of 130 °C. The water generated during the reaction was distilled off, and it was in a full discharge state. Samples were taken during the reaction for gas chromatography analysis. When the mass content of herb alcohol ≤ 0.5%, the reaction was stopped, and after washing with water, 313.28 g of sodium herb alcohol with a content of 94.15% was obtained.

[0068] 178 g of the sodium herb alcohol obtained above and 184 g of 2-fluoro-2-methyl-1-propanol were put into a 1000 mL three-necked flask and reacted at a temperature of 80 °C. Samples were taken during the reaction for gas chromatography analysis. When the mass content of 2-fluoro-2-methyl-1-propanol ≤ 0.5%, the reaction was stopped, and the sodium herb alcohol was removed by washing with water to obtain a crude product with a content of 89.45%. Then, vacuum distillation gave 178.78 g of an intermediate with a content of 97.23%.

[0069] 114 g of the intermediate obtained above, 88 g of methyl propionate and 5 g of dibutyltin oxide were put into a 1000 mL three-necked flask and reacted at a temperature of 150 °C. Samples were taken during the reaction for gas chromatography analysis. When the mass content of the intermediate ≤ 0.5%, the reaction was stopped, and a crude product with a content of 94.28% was obtained. Vacuum distillation gave 122.66 g of galaxolide with a content of 98.23%.

[0070] Example 6

[0071] 312 g of herb alcohol and 144 g of sodium hydroxide were put into a 1000 mL three-necked flask and reacted at a temperature of 130 °C. The water generated during the reaction was distilled off, and it was in a full discharge state. Samples were taken during the reaction for gas chromatography analysis. When the mass content of herb alcohol ≤ 0.5%, the reaction was stopped, and after washing with water, 304.99 g of sodium herb alcohol with a content of 93.02% was obtained.

[0072] 178 g of the above-obtained sodium herbate and 165.60 g of 2-fluoro-2-methyl-1-propanol were added to a 1000 mL three-necked flask and reacted at a temperature of 80 °C. Samples were taken during the reaction for gas chromatography analysis. When the mass content of 2-fluoro-2-methyl-1-propanol ≤ 0.5%, the reaction was stopped. The sodium herbate was removed by washing with water to obtain a crude product with a content of 87.01%. Then, vacuum distillation was carried out to obtain 169.44 g of an intermediate with a content of 97.50%.

[0073] 114 g of the above-obtained intermediate, 79.20 g of methyl propionate and 5 g of dibutyltin oxide were added to a 1000 mL three-necked flask and reacted at a temperature of 150 °C. Samples were taken during the reaction for gas chromatography analysis. When the mass content of the intermediate ≤ 0.5%, the reaction was stopped to obtain a crude product with a content of 93.46%. Vacuum rectification was carried out to obtain 118.15 g of galaxolide with a content of 97.82%.

[0074] Comparative Example 1

[0075] 50 g of herb alcohol and 100 g of toluene solution were added to a 1000 mL round-bottomed flask. After mixing, 20 g of isobutene oxide was added. Then, at a temperature of -10 °C, 1 g of boron trifluoride etherate was added dropwise with stirring. After that, the reaction was carried out at a temperature of 25 °C for 4 h. After the reaction, vacuum rectification was carried out to obtain the product. The product after vacuum rectification was continued to be added with 1 g of boron trifluoride etherate with stirring at a temperature of -10 °C, and then allowed to stand and react at a temperature of 25 °C for 24 h to obtain a crude product with a content of 18.21%. Vacuum rectification was carried out to obtain 18.21 g of an intermediate with a content of 93.11%.

[0076] The above-obtained intermediate was added to a 100 mL round-bottomed flask, and then 10 g of propionic anhydride and 10 g of pyridine were added. After mixing, the reaction was carried out at a temperature of 25 °C for 24 h. After the reaction, vacuum rectification was carried out to obtain 16.11 g of galaxolide with a content of 84%.

[0077] Comparative Example 2

[0078] 50 g of herb alcohol, 20 g of isobutene oxide and 100 g of cyclohexane solution were added to a 1000 mL round-bottomed flask. After cooling in an ice-water bath, 1 g of boron trifluoride etherate was added, and the reaction was carried out in the ice-water bath for 30 min. Then, 1 g of boron trifluoride etherate was added again, and the reaction was continued in the ice-water bath for 3 h. After the reaction, it was washed with a solution prepared with 5 g of sodium hydroxide, and then separated by silica gel column chromatography to obtain 20.22 g of an intermediate with a content of 76%.

[0079] Add the obtained intermediate to a 100 mL round-bottom flask, heat it to 100 °C, then add 10 g of propionic anhydride. After mixing evenly, reflux the mixture for 6 h. After the reaction is completed, perform vacuum distillation to obtain 22.65 g of galaxolide with a content of 69%.

[0080] Calculate the production costs of preparing 1 kg of galaxolide using the preparation methods of Example 1, Comparative Example 1, and Comparative Example 2. Among them, Table 1 shows the production cost of Example 1, Table 2 shows the production cost of Comparative Example 1, and Table 3 shows the production cost of Comparative Example 2.

[0081] Table 1

[0082] Name Unit Consumption (Kg / Kg) Unit Price (Yuan / Kg) Cost (Yuan / Kg) Herbal Alcohol 1.01 100.00 101.00 Sodium Hydroxide 0.39 3.38 1.32 2-Fluoro-2-methyl-1-propanol 0.80 50.00 40.00 Methyl Propionate 0.56 15.50 8.68 Dibutyltin Oxide 0.04 45.00 1.8 Total / / 152.8

[0083] Table 2

[0084] Name Unit Consumption (Kg / Kg) Unit Price (Yuan / Kg) Cost (Yuan / Kg) Herbal Alcohol 3.69 100.00 369.00 Toluene 1 5.00 5 Isobutene Oxide 1.48 200.00 296.00 Boron Trifluoride Diethyl Etherate 0.15 20.00 3.00 Propionic Anhydride 0.74 12.00 8.88 Pyridine 0.74 26.00 19.24 Total / / 701.12

[0085] Table 3

[0086] Name Unit Consumption (Kg / Kg) Unit Price (Yuan / Kg) Cost (Yuan / Kg) Herbal Alcohol 3.20 100.00 320.00 Isobutene Oxide 1.28 200.00 256.00 Cyclohexane 1 7.00 7.00 Boron Trifluoride Diethyl Etherate 0.13 20.00 2.60 Sodium Hydroxide 0.32 3.38 1.08 Propionic Anhydride 0.64 12.00 7.68 Total / / 594.36

[0087] As can be seen from Table 1, Table 2, and Table 3, the production cost of preparing 1 kg of galaxolide using the preparation method of Example 1 is 152.8 yuan, the production cost of preparing 1 kg of galaxolide using the preparation method of Comparative Example 1 is 701.12 yuan, and the production cost of preparing 1 kg of galaxolide using the preparation method of Comparative Example 2 is 594.36 yuan.

[0088] As can be known from Example 2, Example 3, and other examples, when the molar ratio of herb alcohol to strong base is 1:1.2 - 1:2, the content of the herb alcoholate obtained is higher; as can be known from Example 2, Example 3, and other examples, when the molar ratio of the herb alcoholate to the compound shown in the structural formula of Formula (1) is 1:1.2 - 1:2, the content of the intermediate obtained is higher; as can be known from Example 2, Example 3, and other examples, when the molar ratio of the intermediate to methyl propionate is 1:1.2 - 1:2, the content of the crude galaxolide obtained is higher; as can be known from Examples 1 - 6, Comparative Example 1, and Comparative Example 2, the content of the galaxolide obtained by the preparation method of the present invention is higher; as can be known from the comparison of the production costs of Example 1, Comparative Example 1, and Comparative Example 2 in the test examples, the production cost of the galaxolide obtained by the preparation method of the present invention is low.

[0089] The technical features of the above-described embodiments can be combined arbitrarily. For the sake of concise description, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, it should be considered as the scope recorded in this specification.

[0090] The above-described embodiments merely represent several implementation manners of the present invention. Their descriptions are relatively specific and detailed, but they should not be construed as limiting the scope of the invention patent. It should be noted that for those of ordinary skill in the art, without departing from the concept of the present invention, several modifications and improvements can still be made, and these all fall within the protection scope of the present invention. Therefore, the protection scope of the present invention patent shall be subject to the appended claims.

Claims

1. A preparation method of galaxolide, characterized in that, Comprising the following steps: Reacting herb alcohol with a strong base to obtain an herb alcoholate, wherein the reaction temperature is 120°C - 180°C; Reacting the herb alcoholate with a compound having the structural formula shown in formula (1) to generate an intermediate having the structural formula shown in formula (2); Performing a transesterification reaction on the intermediate and methyl propionate under the action of a transesterification catalyst to obtain galaxolide; 、 ， In formula (1), R is a halogen element.

2. The preparation method of galaxolide according to claim 1, characterized in that, The strong base is selected from at least one of potassium hydroxide and sodium hydroxide.

3. The preparation method of galaxolide according to claim 1, characterized in that, The molar ratio of the herb alcohol to the strong base is 1:1 - 1:

5.

4. The preparation method of galaxolide according to claim 1, characterized in that, The compound having the structural formula shown in formula (1) is selected from 2-fluoro-2-methyl-1-propanol.

5. The preparation method of the galaxolide according to claim 1, characterized in that, The molar ratio of the herb alcoholate to the compound having the structural formula shown in formula (1) is 1:1 - 1:

3.

6. The preparation method of the galaxolide according to claim 1, characterized in that, In the step of reacting the herb alcoholate with the compound having the structural formula shown in formula (1), the reaction temperature is 80°C - 120°C.

7. The preparation method of galaxolide according to claim 1, characterized in that, The molar ratio of the intermediate to methyl propionate is 1:1 - 1:

5.

8. The preparation method of galaxolide according to claim 1, characterized in that, In the step of performing a transesterification reaction on the intermediate and methyl propionate under the action of a transesterification catalyst, the reaction temperature is 100°C - 190°C.

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