Method for preparing alpha-phenethyl alcohol

Abstract

The invention discloses a method for preparing alpha-phenethyl alcohol. The method comprises the following steps: reacting acetyl benzene serving as the raw material, alcohol serving as a hydrogen source and supported alkaline earth metallic oxide as a catalyst for 1 to 10 hours at a the reaction temperature of between 60 and 130 DEG C; and after the reaction is finished, processing the reaction solution to obtain alpha-phenethyl alcohol, wherein the alcohol is C1 to C7 fatty alcohol or C3 to C7 alicyclic alcohol; the mole ratio of the acetyl benzene to the alcohol is 1:5-30; the supported alkaline earth metallic oxide consists of a carrier and alkaline earth metallic oxide supported on the carrier; the alkaline metallic earth oxide is MgO, CaO, SrO or BaO; the carrier is active carbon; and the supporting capacity of the alkaline earth metallic oxide is between 0.5 and 15 weight percent based on the mass of the carrier. The method for preparing the alpha-phenethyl alcohol has the advantages of mild required reaction condition, high activity and high selectivity of the catalyst, short reaction time, no other by-products in the reaction and no pollution to the environment, and is anenvironmental-friendly green synthetic route.

Description

(1) Technical field

[0001] The invention relates to a method for preparing α-phenethyl alcohol by using acetophenone as a raw material through hydrogen transfer. (2) Background technology

[0002] α-Phenylethyl alcohol is a representative compound among aromatic alcohols, and it is also an important chemical product, which is widely used in industries such as medicine, fragrance manufacturing, cosmetics, food and fine chemicals. For example, it is widely used in the fragrance manufacturing industry for aroma reconciliation, and as the main component of rose fragrance, for the synthesis of various rose oils and essential oils; in the synthesis of many drugs, α-phenylethanol is an important drug intermediate, such as In the synthesis of ibuprofen sedative drugs, α-phenylethyl alcohol is an important raw material. As an important spice and fine chemical intermediate, α-phenylethyl alcohol is in increasing demand both at home and abroad.

[0003] The method for preparing α-phe...

Examples

preparation example Construction

[0028] Catalyst preparation method:

[0029] Taking 0.5wt% MgO / AC catalyst as an example, the preparation method is: weigh 0.16gMg(NO 3 ) 2 ·6H 2 O was dissolved in 50ml of deionized water to obtain an aqueous solution of magnesium nitrate, and then 5 g of activated carbon support was immersed in the aqueous solution of magnesium nitrate, and the water was evaporated to dryness with a rotary evaporator, and then calcined at 600 ° C for 6 hours to obtain a 0.5wt% MgO / AC catalyst.

[0030] The preparation methods of various catalysts used in the embodiments of the present invention are all operated according to the above method, the difference is to change the raw materials and consumption, see the following table 1 for details:

[0031] catalyst

Embodiment 1

[0033] Add the 0.5g10wt% MgO / AC catalyst prepared by the above-mentioned catalyst preparation method in the 50mL single-necked round bottom flask, 0.24g acetophenone, 3.6g isopropanol (the material mass ratio of feeding intake is acetophenone: isopropanol=1 : 30), connect a condensing tube, the other end of the condensing tube does not need to be sealed, heat in an oil bath at 85°C, and stir with magnetic force at the same time, after reacting for 4 hours, analyze acetophenone and α-phenylethanol in the reaction solution by gas chromatography content, the results are shown in Table 1, the reaction solution was rectified, and the 200-210 ° C fraction was taken to obtain 0.21 g of α-phenylethanol product, with a yield of 92%.

Embodiment 2-4

[0035]Other reaction conditions are as embodiment 1, difference is that embodiment 2 adopts 10wt%CaO / AC catalyst, embodiment 3 has adopted 10wt%SrO / AC catalyst, embodiment 4 has adopted 10wt%BaO / AC catalyst, with gas chromatography Analyze the content of acetophenone and α-phenethyl alcohol in the reaction solution after the reaction finishes, and the results are shown in Table 1.

(1) Technical field

[0001] The invention relates to a method for preparing α-phenethyl alcohol by using acetophenone as a raw material through hydrogen transfer. (2) Background technology

[0002] α-Phenylethyl alcohol is a representative compound among aromatic alcohols, and it is also an important chemical product, which is widely used in industries such as medicine, fragrance manufacturing, cosmetics, food and fine chemicals. For example, it is widely used in the fragrance manufacturing industry for aroma reconciliation, and as the main component of rose fragrance, for the synthesis of various rose oils and essential oils; in the synthesis of many drugs, α-phenylethanol is an important drug intermediate, such as In the synthesis of ibuprofen sedative drugs, α-phenylethyl alcohol is an important raw material. As an important spice and fine chemical intermediate, α-phenylethyl alcohol is in increasing demand both at home and abroad.

[0003] The method for preparing α-phe...

Examples

preparation example Construction

[0028] Catalyst preparation method:

[0029] Taking 0.5wt% MgO / AC catalyst as an example, the preparation method is: weigh 0.16gMg(NO 3 ) 2 ·6H 2 O was dissolved in 50ml of deionized water to obtain an aqueous solution of magnesium nitrate, and then 5 g of activated carbon support was immersed in the aqueous solution of magnesium nitrate, and the water was evaporated to dryness with a rotary evaporator, and then calcined at 600 ° C for 6 hours to obtain a 0.5wt% MgO / AC catalyst.

[0030] The preparation methods of various catalysts used in the embodiments of the present invention are all operated according to the above method, the difference is to change the raw materials and consumption, see the following table 1 for details:

[0031] catalyst

Embodiment 1

[0033] Add the 0.5g10wt% MgO / AC catalyst prepared by the above-mentioned catalyst preparation method in the 50mL single-necked round bottom flask, 0.24g acetophenone, 3.6g isopropanol (the material mass ratio of feeding intake is acetophenone: isopropanol=1 : 30), connect a condensing tube, the other end of the condensing tube does not need to be sealed, heat in an oil bath at 85°C, and stir with magnetic force at the same time, after reacting for 4 hours, analyze acetophenone and α-phenylethanol in the reaction solution by gas chromatography content, the results are shown in Table 1, the reaction solution was rectified, and the 200-210 ° C fraction was taken to obtain 0.21 g of α-phenylethanol product, with a yield of 92%.

Embodiment 2-4

[0035]Other reaction conditions are as embodiment 1, difference is that embodiment 2 adopts 10wt%CaO / AC catalyst, embodiment 3 has adopted 10wt%SrO / AC catalyst, embodiment 4 has adopted 10wt%BaO / AC catalyst, with gas chromatography Analyze the content of acetophenone and α-phenethyl alcohol in the reaction solution after the reaction finishes, and the results are shown in Table 1.

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