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Production method of 2-campholenic propyl aldehyde

A kind of campholenyl propionaldehyde, production method technology, applied in chemical instruments and methods, carbon-based compound preparation, organic compound preparation and other directions, can solve the problems of affecting product quality, serious side reactions, difficult to purify, etc. The environment is favorable, the reaction speed is fast, and the effect of removing impurities that are difficult to separate

Active Publication Date: 2013-12-18
广州百花香料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003]Using borneol and propionaldehyde for aldehyde condensation, the traditional aldol condensation uses a strong base as a catalyst with low yield, serious side reactions, and a large amount of Miscellaneous products (such as US4052341, DE2827957, Zhao 55-36423), resulting in mixed products, difficult to purify, and affecting product quality
There are also carbonates as basic catalysts, which are reacted in a weakly basic system by transferring catalysts (such as CN 101891594 B). Although there is a certain improvement over the traditional method, the process is more complicated

Method used

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  • Production method of 2-campholenic propyl aldehyde

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] In a 2-liter reactor, add 200 g of borneolenal, 240 g of methanol, and 8 g of proline catalyst, stirring and heating to maintain 40° C. Weigh 128g of n-propanal, add dropwise in two batches, the first batch is 80g, the second batch is 48g, after the temperature of the stirring solution is kept constant at 40°C, start to add the first batch of n-propanal, control the dropping time for 3hr, drop After completion, continue to stir the reaction to keep the temperature at 40° C. for 1 hr, add the second batch of n-propionaldehyde dropwise, and control the dropping time for 1 hr. After the dropwise addition was completed, it was heated to 60° C., and the reaction was continued for 2 hours. After the reaction, the solvent was recovered, neutralized and washed with water to obtain 276 g of crude product of 2-borneolenyl propionaldehyde, with a content of 72%, and 195 g of the product was recovered, separated and purified, with a content of 94%, and a product yield of 97.5% . ...

Embodiment 2

[0040] In a 2-liter reactor, add 200 g of borneolenal, 240 g of methanol, and 4 g of proline catalyst, stirring and heating to maintain 45° C. Weigh 128g of n-propanal, add dropwise in two batches, the first batch is 88g, the second batch is 40g, after the temperature of the stirring solution is kept at 40°C, start to drop the first batch of n-propanal, control the dropping time for 3.5hr, drop After the addition, continue to stir the reaction to keep the temperature at 40° C. for 1 hr, add the second batch of n-propionaldehyde dropwise, and control the dropping time for 1 hr. After the dropwise addition was completed, it was heated to 65° C., and the reaction was continued for 3 hours. After the reaction, the solvent was recovered, neutralized and washed with water to obtain 270 g of the crude product of 2-borneolenyl propionaldehyde, with a content of 69%, and 185 g of the product was recovered after separation and purification, with a content of 94% and a yield of 92.5%. ....

Embodiment 3

[0042]In a 2-liter reactor, add 200 g of borneolenal, 200 g of ethanol, and 8 g of proline catalyst, stirring and heating to maintain 50° C. Weigh 180g of n-propanal, add it dropwise in two batches, the first batch is 120g, the second batch is 60g, after the temperature of the stirring liquid is kept constant at 50°C, start to drop the first batch of n-propanal, control the dropping time for 5hr, drop After completion, continue to stir the reaction to keep the temperature at 50° C. for 1 hr, add the second batch of n-propanal dropwise, and control the dropping time for 1.5 hr. After the dropwise addition was completed, it was heated to 70° C., and the reaction was continued for 2 hours. After the reaction, the solvent was recovered, neutralized and washed with water to obtain 292 g of the crude product of 2-borneolenyl propionaldehyde, with a content of 58%, and 179 g of the product was recovered, separated and purified, with a content of 93%, and a product yield of 89.5% . ...

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Abstract

The invention discloses a production method of 2-campholenic propyl aldehyde. The production method of the 2-campholenic propyl aldehyde comprises the following steps: adding campholenic aldehyde, n-propanal, methanol or ethanol and a catalyst, namely proline or a derivative of the proline into a reaction kettle, performing direct reaction at a certain reaction temperature, and performing neutralization, washing with water and purification, thereby obtaining a 2-campholenic propyl aldehyde product. According to the synthesis production process provided by the invention, a one-pot method reaction technology is adopted, the proline catalyst is used for replacing a traditional strong base catalyst, byproducts brought by a traditional process are reduced, the product yield and the product quality are further improved, the environmental pollution is reduced, and the effects of reducing the production cost, and reducing the environmental protection cost are also achieved.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and specifically refers to a production method of 2-borneolenyl propanal. Background technique [0002] 2-bornylidene propanal can be used as a raw material for the synthesis of Sandalmysore core, and it is an important intermediate product for the synthesis of fragrance 2-bornylidene propanol. Bradman Sandalwood (2-Bornylidene Propanol) has a strong woody aroma reminiscent of natural sandalwood. It is used in daily chemical essence formulations such as soap, shampoo, cosmetics, etc. [0003] Using bornaldehyde and propionaldehyde for aldehyde condensation, the traditional aldol condensation uses a strong base as a catalyst with low yield, serious side reactions, and a large amount of miscellaneous products (such as US4052341, DE2827957, Zhao 55-36423), resulting in The product is mixed, it is difficult to purify, and the quality of the product is affected. There is also a method that u...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/225C07C45/74B01J31/04
Inventor 焦亦正张建斌
Owner 广州百花香料股份有限公司
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