Preparation method of musk romain

Abstract

The present invention relates to a method for preparing musk romain, comprising: subjecting herb alcohol to an ester exchange reaction with a halogenated ester having a structural formula as shown in formula (1) under the action of an ester exchange catalyst to obtain an intermediate having a structural formula as shown in formula (2), wherein R is a halogen element; and subjecting the intermediate to a reaction with a propionate under the action of a phase transfer catalyst to obtain musk romain. The method for preparing musk romain of the present invention has easy-to-obtain raw materials, low production cost, and high yield of musk romain.

Description

Technical Field

[0001] The invention relates to the technical field of perfumes, in particular to a preparation method of musk romain. Background Art

[0002] Roman musk is a musk with a very delicate aroma. Compared with sea musk, it has less fruity and sunflower scent, but when dried, it has a longer lasting fragrance and a stronger aroma. It can be used to scent perfumes, toiletries and daily necessities.

[0003] There are two main traditional production processes for Roman Musk: one is to obtain Roman Musk by esterification reaction of herb alcohol with 2-(propionyloxy)acetic acid. However, the raw material 2-(propionyloxy)acetic acid used in the synthesis of this method is expensive and the production cost is high; the other is to obtain Roman Musk by esterification reaction of herb alcohol with chloroacetic acid first and then with propionic acid. However, the yield of Roman Musk by this method is low. Summary of the invention

[0004] Based on this, it is necessary to provide a method for preparing Roman Musk in order to solve the above problems. The raw materials of the preparation method are easily available, the production cost is low, and the yield of Roman Musk is high.

[0005] A method for preparing musk romain, comprising the following steps:

[0006] The herb alcohol and the halogenated ester represented by the structural formula (1) are subjected to an ester exchange reaction under the action of an ester exchange catalyst to obtain an intermediate represented by the structural formula (2);

[0007] The intermediate is reacted with propionate under the action of a phase transfer catalyst to obtain musk de romane;

[0008]

[0009] Wherein, R is a halogen element.

[0010] In one embodiment, the halogenated ester is selected from ethyl chloroacetate.

[0011] In one embodiment, the molar ratio of the herb alcohol to the halogenated ester is 1:1-1:2.

[0012] 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.

[0013] In one embodiment, in the step of subjecting the herb alcohol to transesterification reaction with the halogenated ester represented by the structural formula (1) under the action of a catalyst, the reaction temperature is 80° C.-180° C.

[0014] In one embodiment, after the step of subjecting the herb alcohol to transesterification with the halogenated ester represented by the structural formula (1) under the action of a catalyst, the intermediate is obtained by vacuum distillation.

[0015] In one embodiment, the propionate salt is selected from sodium propionate.

[0016] In one embodiment, the molar ratio of the intermediate to the propionate is 1:1-1:2.

[0017] In one embodiment, the phase transfer catalyst is selected from at least one of benzyltriethylammonium chloride, tetrabutylammonium bromide, tetrabutylammonium chloride, tetrabutylammonium hydrogen sulfate, chain polyethylene glycol, 18-crown ether-6, and pyridine.

[0018] In one embodiment, in the step of reacting the intermediate with propionate in the presence of a phase transfer catalyst, the reaction temperature is 100°C-190°C.

[0019] In the preparation method of musk romana of the present invention, herb alcohol is used as a raw material, and musk romana is generated through an ester exchange reaction and a phase transfer catalytic reaction. The raw materials and reactants are widely available and inexpensive. Meanwhile, since the phase transfer catalytic reaction does not require that the intermediate and the propionate be dissolved in the same solvent, it is not necessary to use expensive anhydrous solvents or non-protonic solvents during the reaction process. The phase transfer catalyst is widely available and inexpensive, which further reduces the production cost. In addition, the catalysts for the ester exchange reaction and the phase transfer catalytic reaction have high catalytic efficiency, fast reaction speed, good reaction selectivity and high conversion rate, thereby reducing the generation of by-products, so that the yield of musk romana is high and the production cost is low. DETAILED DESCRIPTION

[0020] For ease of understanding of the present invention, the present invention will be described more fully 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, the purpose of providing these embodiments is to make the understanding of the disclosure of the present invention more thorough and comprehensive.

[0021] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those commonly understood by those skilled in the art of the present invention. The terms used herein in the specification of the present invention 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 related listed items.

[0022] The preparation method of musk romain provided by the present invention comprises the following steps:

[0023] S1, performing an ester exchange reaction between herb alcohol and a halogenated ester represented by the structural formula (1) under the action of an ester exchange catalyst to obtain an intermediate represented by the structural formula (2), and the reaction equation is as follows:

[0024]

[0025] Wherein, R is a halogen element, and the halogen element is selected from chlorine, bromine, iodine, etc. Further, the halogenated ester is preferably ethyl chloroacetate.

[0026] The present invention does not limit the source of herb alcohol, and commercially available herb alcohol can be directly purchased, or it can be obtained by hydrolyzing avermectin ester under alkaline conditions.

[0027] 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, preferably potassium carbonate.

[0028] During the transesterification reaction, in addition to the intermediates, ethanol is also produced. However, due to the low boiling point of ethanol, it will be directly evaporated from the reaction system during the reaction. In addition, since the transesterification reaction is a reversible reaction, the evaporation of ethanol will cause the reaction to move towards the direction of generating intermediates, thereby increasing the reaction rate and the yield of the intermediates.

[0029] In order to better generate the intermediate with the structural formula shown in formula (2), in one embodiment, the molar ratio of the herb alcohol to the halogenated ester is 1:1-1:2, preferably 1:1.2-1:1.5.

[0030] In one embodiment, the molar ratio of the transesterification catalyst to the herb alcohol is 1:1.2-1:1.5.

[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 conducting an ester exchange reaction between the herb alcohol and the halogenated ester represented by the structural formula (1) under the action of a catalyst, the reaction temperature is 80°C-180°C, preferably 110°C-150°C.

[0032] Since ethanol has been evaporated during the reaction, only a small amount of ethanol and unreacted halogenated ester remain after the reaction is completed, and the remaining ethanol and unreacted halogenated ester have lower boiling points than the intermediate. Therefore, the intermediate can be obtained by vacuum distillation after the reaction is completed.

[0033] S2, reacting the intermediate with propionate in the presence of a phase transfer catalyst to obtain musk de romane.

[0034] Wherein, the propionate is selected from at least one of sodium propionate, potassium propionate, and lithium propionate, preferably sodium propionate; the phase transfer catalyst can be an onium salt, a polyether, or a calixarene catalyst, specifically, can be selected from at least one of benzyltriethylammonium chloride, tetrabutylammonium bromide, tetrabutylammonium chloride, tetrabutylammonium hydrogen sulfate, chain polyethylene glycol, 18-crown ether-6, and pyridine, preferably tetrabutylammonium hydrogen sulfate.

[0035] Taking sodium propionate as an example, the reaction formula of the intermediate and sodium propionate is:

[0036]

[0037] In step S2, since the intermediate and propionate do not react when the phase transfer catalyst is not added, there is no restriction on the order of adding the intermediate and propionate. The intermediate can be added first and then the propionate, or the propionate can be added first and then the intermediate, or both can be added simultaneously.

[0038] In order to better produce Roman musk, in one embodiment, the molar ratio of the intermediate to the propionate is 1:1-1:2, preferably 1:1.2-1:1.5.

[0039] In one embodiment, the molar ratio of the phase transfer catalyst to the intermediate is 1:1.2-1:1.5.

[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 intermediate with propionate under the action of a phase transfer catalyst, the reaction temperature is 100°C-190°C, preferably 130°C-150°C.

[0041] Since the intermediate and propionate undergo a phase transfer catalytic reaction, the reactants are immiscible, and the generated Roman Musk is immiscible with other chemical substances in the entire reaction system, so after the reaction is completed, other chemical substances in the entire reaction system can be removed by washing with water, and only Roman Musk is retained, which is easy to operate. At the same time, since the phase transfer catalytic reaction does not require the intermediate and propionate to be dissolved in the same solvent, expensive anhydrous solvents or non-protonic solvents do not need to be used during the reaction process, and the sources of propionate and phase transfer catalysts are wide and cheap, which further reduces the production cost of Roman Musk.

[0042] It should be noted that the crude product of musk desmoss is obtained by reacting the intermediate with propionate in the presence of a phase transfer catalyst, and musk desmoss is obtained by vacuum distillation or the like.

[0043] In the preparation method of musk romain of the present invention, herb alcohol is used as a raw material, and musk romain is generated through ester exchange reaction and phase transfer catalytic reaction. The raw materials and reactants are easily available and inexpensive, and the catalyst cost of the ester exchange reaction and the phase transfer catalytic reaction is low and the catalytic efficiency is high, the reaction speed is fast, the reaction selectivity is good and the conversion rate is high, thereby reducing the generation of by-products, so that the yield of musk romain is high and the production cost is low.

[0044] Hereinafter, the preparation method of the musk deodorant will be further described through the following specific examples.

[0045] Example 1

[0046] 312g of herb alcohol, 300g of ethyl chloroacetate and 4g of potassium carbonate were put into a 1000mL three-necked flask, and an ester exchange reaction was carried out at a temperature of 130°C. The ethanol produced during the reaction was evaporated, and the reaction was in a full discharge state. During the reaction, a sample was taken for gas chromatography analysis. When the mass content of herb alcohol was ≤0.5%, the reaction was stopped, and the crude product content was 95.65%. Ethanol and ethyl chloroacetate were removed by vacuum distillation, and then vacuum distillation was performed to obtain 421.63g of an intermediate with a content of 99.98%.

[0047] 232g of the intermediate obtained above, 200g of toluene, 116g of sodium propionate and 5g of tetrabutylammonium hydrogen sulfate were put into a 1000mL 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 was ≤0.5%, the reaction was stopped. The crude product had a content of 93.24%. Sodium propionate and sodium chloride were removed by washing with water, and then vacuum distillation was performed to obtain 239.16g of Roman Musk with a content of 98.39%.

[0048] Example 2

[0049] 312g of herb alcohol, 244g of ethyl chloroacetate and 4g of potassium carbonate were put into a 1000mL three-necked flask, and an ester exchange reaction was carried out at a temperature of 80°C. The ethanol produced during the reaction was evaporated, and the reaction was in a full discharge state. During the reaction, samples were taken for gas chromatography analysis. When the mass content of herb alcohol was ≤0.5%, the reaction was stopped, and the crude product content was 76.18%. Ethanol and ethyl chloroacetate were removed by vacuum distillation, and then vacuum distillation was performed to obtain 335.88g of an intermediate with a content of 99.84%.

[0050] 232g of the intermediate obtained above, 200g of toluene, 116g of sodium propionate and 5g of tetrabutylammonium hydrogen sulfate were put into a 1000mL three-necked flask and reacted at a temperature of 100°C. Samples were taken during the reaction for gas chromatography analysis. When the mass content of the intermediate was ≤0.5%, the reaction was stopped. The crude product had a content of 83.15%. Sodium propionate and sodium chloride were removed by washing with water, and then vacuum distillation was performed to obtain 213.28g of Roman Musk with a content of 98.18%.

[0051] Example 3

[0052] 312g of herb alcohol, 488g of ethyl chloroacetate and 4g of potassium carbonate were put into a 1000mL three-necked flask, and an ester exchange reaction was carried out at a temperature of 130°C. The ethanol produced during the reaction was evaporated, and the reaction was in a full discharge state. During the reaction, samples were taken for gas chromatography analysis. When the mass content of herb alcohol was ≤0.5%, the reaction was stopped, and the crude product content was 88.14%. Ethanol and ethyl chloroacetate were removed by vacuum distillation, and then vacuum distillation was performed to obtain 385.60g of an intermediate with a content of 99.44%.

[0053] 232g of the intermediate obtained above, 200g of toluene, 116g of sodium propionate and 5g of tetrabutylammonium hydrogen sulfate were put into a 1000mL three-necked flask and reacted at a temperature of 170°C. Samples were taken during the reaction for gas chromatography analysis. When the mass content of the intermediate was ≤0.5%, the reaction was stopped. The crude product had a content of 83.98%. Sodium propionate and sodium chloride were removed by washing with water, and then vacuum distillation was performed to obtain 215.46g of Roman Musk with a content of 98.51%.

[0054] Example 4

[0055] 312g of herb alcohol, 300g of ethyl chloroacetate and 4g of potassium carbonate were put into a 1000mL three-necked flask, and an ester exchange reaction was carried out at a temperature of 130°C. The ethanol produced during the reaction was evaporated, and the product was in a full discharge state. Samples were taken during the reaction for gas chromatography analysis. When the mass content of herb alcohol was ≤0.5%, the reaction was stopped, and the crude product content was 95.12%. Ethanol and ethyl chloroacetate were removed by vacuum distillation, and then vacuum distillation was performed to obtain 419.29g of an intermediate with a content of 99.91%.

[0056] 232g of the intermediate obtained above, 200g of toluene, 96g of sodium propionate and 5g of tetrabutylammonium hydrogen sulfate were put into a 1000mL three-necked flask and reacted at a temperature of 190°C. Samples were taken during the reaction for gas chromatography analysis. When the mass content of the intermediate was ≤0.5%, the reaction was stopped. The crude product had a content of 76.28%. Sodium propionate and sodium chloride were removed by washing with water, and then vacuum distillation was performed to obtain 195.66g of Roman musk with a content of 98.18%.

[0057] Example 5

[0058] 312g of herb alcohol, 300g of ethyl chloroacetate and 4g of potassium carbonate were put into a 1000mL three-necked flask, and an ester exchange reaction was carried out at a temperature of 130°C. The ethanol produced during the reaction was evaporated, and the product was in a full discharge state. During the reaction, a sample was taken for gas chromatography analysis. When the mass content of herb alcohol was ≤0.5%, the crude product content was 94.98%, the reaction was stopped, and the ethanol and ethyl chloroacetate were removed by vacuum distillation, and then vacuum distillation was performed to obtain 412.67g of an intermediate with a content of 99.84%.

[0059] 232g of the intermediate obtained above, 200g of toluene, 192g of sodium propionate and 5g of tetrabutylammonium hydrogen sulfate were put into a 1000mL three-necked flask and reacted at a temperature of 170°C. Samples were taken during the reaction for gas chromatography analysis. When the mass content of the intermediate was ≤0.5%, the reaction was stopped. The crude product had a content of 85.22%. Sodium propionate and sodium chloride were removed by washing with water, and then vacuum distillation was performed to obtain 218.59g of Roman musk with a content of 98.42%.

[0060] Example 6

[0061] 312g of herb alcohol, 440g of ethyl chloroacetate and 4g of potassium carbonate were put into a 2000mL three-necked flask, and an ester exchange reaction was carried out at a temperature of 130°C. The ethanol produced during the reaction was evaporated, and the reaction was in a full discharge state. During the reaction, samples were taken for gas chromatography analysis. When the mass content of herb alcohol was ≤0.5%, the reaction was stopped, and the crude product content was 89.52%. Ethanol and ethyl chloroacetate were removed by vacuum distillation, and then vacuum distillation was performed to obtain 394.60g of an intermediate with a content of 99.83%.

[0062] 232g of the intermediate obtained above, 200g of toluene, 115.2g of sodium propionate and 5g of tetrabutylammonium hydrogen sulfate were put into a 1000mL 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 was ≤0.5%, the reaction was stopped. The crude product had a content of 94.05%. Sodium propionate and sodium chloride were removed by washing with water, and then vacuum distillation was performed to obtain 240.25g of musk roman with a content of 98.17%.

[0063] Example 7

[0064] 312g of herb alcohol, 366g of ethyl chloroacetate and 4g of potassium carbonate were put into a 1000mL three-necked flask, and an ester exchange reaction was carried out at a temperature of 110°C. The ethanol produced during the reaction was evaporated, and the reaction was in a full discharge state. During the reaction, a sample was taken for gas chromatography analysis. When the mass content of herb alcohol was ≤0.5%, the reaction was stopped, and the crude product content was 93.09%. Ethanol and ethyl chloroacetate were removed by vacuum distillation, and then vacuum distillation was performed to obtain 403.55g of an intermediate with a content of 99.84%.

[0065] 232g of the intermediate obtained above, 200g of toluene, 116g of sodium propionate and 5g of tetrabutylammonium hydrogen sulfate were put into a 1000mL 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 was ≤0.5%, the reaction was stopped. The crude product had a content of 94.79%. Sodium propionate and sodium chloride were removed by washing with water, and then vacuum distillation was performed to obtain 237.15g of Roman Musk with a content of 98.22%.

[0066] Example 8

[0067] 312g of herb alcohol, 293g of ethyl chloroacetate and 4g of potassium carbonate were put into a 1000mL three-necked flask, and an ester exchange reaction was carried out at a temperature of 150°C. The ethanol produced during the reaction was evaporated, and the reaction was in a full discharge state. During the reaction, samples were taken for gas chromatography analysis. When the mass content of herb alcohol was ≤0.5%, the reaction was stopped, and the crude product content was 95.13%. Ethanol and ethyl chloroacetate were removed by vacuum distillation, and then vacuum distillation was performed to obtain 414.02g of an intermediate with a content of 99.84%.

[0068] 232g of the intermediate obtained above, 200g of toluene, 144g of sodium propionate and 5g of tetrabutylammonium hydrogen sulfate were put into a 1000mL 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 was ≤0.5%, the reaction was stopped. The crude product had a content of 92.63%. Sodium propionate and sodium chloride were removed by washing with water, and then vacuum distillation was performed to obtain 243.18g of Roman Musk with a content of 98.55%.

[0069] Example 9

[0070] 312g of herb alcohol, 400g of ethyl bromoacetate and 4g of sodium carbonate were put into a 1000mL three-necked flask, and an ester exchange reaction was carried out at a temperature of 120°C. The ethanol produced during the reaction was evaporated, and the reaction was in a full discharge state. During the reaction, a sample was taken for gas chromatography analysis. When the mass content of herb alcohol was ≤0.5%, the reaction was stopped, and the crude product content was 93.99%. Ethanol and ethyl fluoroacetate were removed by vacuum distillation, and then vacuum distillation was performed to obtain 406.78g of an intermediate with a content of 99.87%.

[0071] 232g of the intermediate obtained above, 200g of toluene, 135g of potassium propionate and 5g of 18-crown ether-6 were put into a 1000mL three-necked flask and reacted at a temperature of 140°C. Samples were taken during the reaction for gas chromatography analysis. When the mass content of the intermediate was ≤0.5%, the reaction was stopped. The crude product content was 92.83%. The potassium propionate and potassium chloride were removed by washing with water, and then vacuum distillation was performed to obtain 229.61g of musk roman with a content of 98.11%.

[0072] Comparative Example 1

[0073] 3 g of herb alcohol, 2.9 g of 2-(propionyloxy)acetic acid and 1.52 g of pyridine were dissolved in 70 mL of diethyl ether. Then, the reaction mixture was stirred for 30 min and then 2.9 g of 2-(propionyloxy)acetic acid was added. After 1 h of reaction, 5 mL of aqueous hydrogen chloride was added to stop the reaction. The reaction mixture was then extracted with diethyl ether. After flash chromatography of the extract and concentration of the solution, the mixture was heated at 120 °C and 9 × 10 2 Pa, and distilled the concentrated reaction product to obtain 4.12 g of musk romain with a content of 79.5%.

[0074] Test Case

[0075] Using the preparation methods of Example 1 and Comparative Example 1, 1 kg of musk desmodium romain was prepared respectively, and the production costs were calculated. The production cost of Example 1 is shown in Table 1, and the production cost of Comparative Example 1 is shown in Table 2.

[0076] Table 1

[0077]

[0078]

[0079] Table 2

[0080] name Unit consumption (Kg / Kg) Unit price (yuan / Kg) Cost (yuan / Kg) Herb alcohol 0.91 100.00 91.00 2-(Propionyloxy)acetic acid 1.77 50 88.50 Pyridine 0.46 26 11.96 Diethyl ether 2.13 10 21.30 Hydrogen chloride 1.52 0.39 1.26 Ether 2.13 10 21.3 total / / 235.32

[0081] It can be seen from Table 1 and Table 2 that the production cost of producing 1 kg of Roman Musk by the preparation method of Example 1 is 90.01 yuan, and the production cost of producing 1 kg of Roman Musk by the preparation method of Comparative Example 1 is 235.32 yuan.

[0082] Comparative Example 2

[0083] 300 g of herb alcohol, 321 g of chloroacetic acid and 42 g of 4-dimethylaminopyridine were put into 4500 mL of dichloromethane solution. At 0°C, in a nitrogen environment, 25.8 g of N,N-dicyclohexylcarbodiimide was added to the above solution. The mixture was stirred at 25°C for 1 hour to react. After the reaction, the precipitate was vacuum filtered. The filtered filtrate was concentrated under reduced pressure. The residue obtained by concentration was purified by silica gel. The mobile phase during the purification process was a mixture of pentane and ether. The volume ratio of pentane to ether was 19:1. 420 g of an intermediate with a content of 83% was obtained.

[0084] 200 g of the intermediate obtained above, 64 g of propionic acid, 12 g of potassium carbonate and 135 g of sodium bromide were placed in a mixture of 1600 mL of ether and 400 mL of dioxane, and refluxed for 24 hours to react. After the reaction, it was extracted with ether, then washed with water and sodium chloride solution, dried with magnesium sulfate after washing, and the solvent was evaporated under reduced pressure. Purification was performed on silica gel. During the purification process, the mobile phase was a mixture of pentane and ether, and the volume ratio of pentane to ether was 9:1, and 74 g of musk with a content of 64% was obtained.

[0085] 1 kg of musk deodorant was prepared by the preparation method of Comparative Example 2, and its production cost was calculated by the production cost calculation method of the above test example. The result is shown in Table 3, which is 498 yuan.

[0086] Table 3

[0087] name Unit consumption (Kg / Kg) Unit price (yuan / Kg) Cost (yuan / Kg) Herb alcohol 3.08 100.00 308.00 Chloroacetic acid 3.33 4.00 13.32 4-Dimethylaminopyridine 0.44 130.00 57.20 Dichloromethane 0.46 2.50 1.15 N,N-Dicyclohexylcarbodiimide 0.27 110.00 29.70 Ether 0.35 10.00 3.50 Propionic acid 1.39 3.50 4.87 Potassium carbonate 0.26 10.00 2.60 Sodium bromide 2.94 26.00 76.44 Dioxane 0.09 13.00 1.17 Sodium chloride 0.01 1.90 0.02 Magnesium sulfate 0.01 3.00 0.03 total / / 498.00

[0088] It can be seen from Examples 1, 7, 8 and other examples that when the molar ratio of herb alcohol to the halogenated ester with the structural formula (1) is 1:1.2-1:1.5, the content of the obtained intermediate is higher; it can be seen from Examples 1, 6, 7, 8 and other examples that when the molar ratio of the intermediate to the propionate is 1:1.2-1:1.5, the content of the obtained musk de romana is higher; it can be seen from Examples 1-9 and Comparative Examples 1 and 2 that the content of musk de romana obtained by the preparation method of the present invention is higher; it can be seen from the comparison of the production costs of Example 1, Comparative Example 1 and Comparative Example 2 in the test example that the cost of musk de romana obtained by the preparation method of the present invention is low.

[0089] The technical features of the above-described embodiments may be arbitrarily combined. To make the description concise, not all possible combinations of the technical features in the above-described embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0090] The above-mentioned embodiments only express several implementation methods of the present invention, and the descriptions thereof are relatively specific and detailed, but they cannot be understood as limiting the scope of the invention patent. It should be pointed out that, for ordinary technicians in this field, several variations and improvements can be made without departing from the concept of the present invention, and these all belong to the protection scope of the present invention. Therefore, the protection scope of the patent of the present invention shall be subject to the attached claims.

Claims

1. A method for preparing musk romain, characterized in that: The steps include: The herb alcohol and the halogenated ester represented by the structural formula (1) are subjected to an ester exchange reaction under the action of an ester exchange catalyst to obtain an intermediate represented by the structural formula (2), wherein the ester exchange catalyst is at least one selected from the group consisting of sodium carbonate, potassium carbonate, sodium methoxide methanol solution, p-toluenesulfonic acid, di-n-butyltin oxide, and isopropyl titanate; The intermediate is reacted with propionate under the action of a phase transfer catalyst to obtain musk de romane; Wherein, R is a halogen element, the halogen element is selected from chlorine or bromine, the propionate is selected from sodium propionate, and the phase transfer catalyst is selected from at least one of benzyltriethylammonium chloride, tetrabutylammonium bromide, tetrabutylammonium chloride, tetrabutylammonium hydrogen sulfate, chain polyethylene glycol, 18-crown ether-6, and pyridine.

2. The method for preparing musk Roman according to claim 1, characterized in that: The halogenated ester is selected from ethyl chloroacetate.

3. The method for preparing musk Roman according to claim 1, characterized in that: The molar ratio of the herb alcohol to the halogenated ester is 1:1-1:

2.

4. The method for preparing musk Roman according to claim 1, characterized in that: In the step of subjecting the herb alcohol to transesterification reaction with the halogenated ester represented by the structural formula (1) under the action of a catalyst, the reaction temperature is 80°C-180°C.

5. The method for preparing musk Roman according to claim 1, characterized in that: After the step of subjecting the herb alcohol to transesterification with the halogenated ester represented by the structural formula (1) under the action of a catalyst, the intermediate is obtained by vacuum distillation.

6. The method for preparing musk Roman according to claim 1, characterized in that: The molar ratio of the intermediate to the propionate is 1:1-1:

2.

7. The method for preparing musk Roman according to claim 1, characterized in that: In the step of reacting the intermediate with propionate under the action of a phase transfer catalyst, the reaction temperature is 100°C-190°C.

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