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Method of catalytically synthesizing helional by utilizing composite catalyst

A composite catalyst, the technology of new jasmonaldehyde, which is applied in chemical instruments and methods, physical/chemical process catalysts, organic chemistry and other directions, can solve the problems of low application rate, many side reactions, difficult separation, etc., and achieves less by-product generation. , The effect of less three wastes and mild reaction conditions

Active Publication Date: 2015-04-29
ANHUI HYEA AROMAS
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Problems solved by technology

Wherein there are multiple methods for the condensation reaction with propionaldehyde, such as the ethanol solution of common liquid alkali, but this method has more side reactions, lower yield, and the catalyst is difficult to recycle, the aftertreatment is complicated, and produces a large amount of waste water; Synthesis of Xinyang jasmonal by transfer catalysis has the disadvantages of high price of phase transfer catalyst and difficulty in separation. The phase transfer catalyst remaining in the final product affects the quality of the final perfume; the anion exchange resin method has mild reaction conditions and easy separation of products, but The preparation process of the catalyst required for the reaction is complicated, the regeneration of the anion exchange resin is complicated, and the application rate is low
[0004] Patent CN102503927 discloses a method for preparing Xinyang Jasmonal from 4-(2-methylallyl)-1,2-benzenediol. Although the method can realize the effective utilization of by-products and turn waste into treasure, However, in the preparation of 2-methyl-3-(3,4-methylenedioxyphenyl) propanol, column chromatography is required to obtain the target product, which is not suitable for industrial production and reduces its industrial application value

Method used

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  • Method of catalytically synthesizing helional by utilizing composite catalyst

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Embodiment 1

[0021] Add piperonal and organic solvent ethanol in the reactor, then add the catalyst Pd-KF / Al in the reactor 2 o 3 , heated to 50-80°C, add propionaldehyde dropwise to the reactor, keep warm for 2 hours after dropping, pass hydrogen into the reactor, adjust the pressure to 0.3MPa, react for 3 hours, then reduce the pressure of the reactor to normal pressure, filter and recover Catalyst, the filtrate was rotary evaporated to remove the solvent, and the obtained liquid was 5.6 g of the target product, with a yield of 87.5% and a purity of 94.1%.

[0022] Product IR: ν max / cm -1 : 3066 (C-H on the benzene ring), 1608, 1490, 1450 (C=C on the benzene ring), 2920, 2850 (R-CH / CH 2 ), 1733 (C=O), 1040 (C-O).

[0023] The raw materials are prepared with the molar ratio of piperonal to propionaldehyde = 1:1.3.

[0024] The catalyst is Pd-KF / Al 2 o 3 , wherein the Pd content is 0.6wt%, n(Pd):n(KF)=1:10, and the catalyst mass is 0.6% of the piperonal mass.

[0025] The quality ...

Embodiment 2-9

[0027] The preparation process is the same as in Example 1, but the ratio of raw materials, the amount of catalyst, the condensation reaction time, the reduction reaction time or the hydrogen pressure are changed, so that the yield and purity change accordingly. The details are as shown in Table 1:

[0028] The reaction condition of table 1 embodiment 1-9 and result statistical table

[0029]

[0030] As can be seen from Table 1, the yield of embodiment 1-9 is more than 75%, and the purity is about 90%, and wherein embodiment 9 has used the composite catalyst that embodiment 1 reclaims, and its yield still can reach 78.1%, and The recycling of the composite catalyst is not only environmentally friendly, but also can reduce production costs.

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Abstract

The invention discloses a method of catalytically synthesizing helional by utilizing a composite catalyst and relates to the technical field of organic catalytic synthesis. The method comprises the following steps: carrying out condensation reaction on piperonal and propionaldehyde under the action of the composite catalyst firstly to prepare piperonylene propanal, then carrying out reduction reaction on the piperonylene propanal and hydrogen to prepare the helional serving as a target product. The method has the characteristics of mild reaction conditions, simpleness in operation, high selectivity and high yield. According to the method disclosed by the invention, the formation amounts of by-product and three wastes are small; as the prepared composite catalyst can be reused, the method is green and environmentally friendly and is capable of lowering the production cost.

Description

Technical field: [0001] The invention relates to the technical field of organic catalytic synthesis, in particular to a method for catalytically synthesizing Xinyangjasmonal with a composite catalyst. Background technique: [0002] Xinyang jasmonal, the chemical name is 2-methyl-3-(3,4-methylenedioxyphenyl) propionaldehyde, is a particularly valuable synthetic fragrance, which has the aroma of new mow grass and lilac , It also has the floral fragrance of ozone head fragrance, and is widely used in the deployment of various soap essences and cosmetic essences. Famous perfumes in the world contain Xinyang jasmonal. Xinyang jasmonal also has bactericidal activity, is highly effective, safe, and has no side effects on the human body, so it can be used in food and oral care products. [0003] In the prior art, the method for synthesizing Xinyangjasmonal is mainly to use the new Yangjasmonal as a raw material, undergo an aldol condensation reaction with propionaldehyde, and fina...

Claims

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Application Information

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IPC IPC(8): C07D317/54B01J27/13
CPCB01J27/13C07D317/54
Inventor 汪民富董金龙王天义徐基龙
Owner ANHUI HYEA AROMAS
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