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Production method of 2-pentylidene cyclopentanone

A technology for the production of pentylidene cyclopentanone and its production method, which is applied in chemical instruments and methods, preparation of carbon-based compounds, preparation of organic compounds, etc., can solve problems such as large loss of raw materials, long process flow, cumbersome preparation process, etc., and achieve Short process flow, simple process flow and simple post-processing effect

Active Publication Date: 2013-04-24
HUAIAN WAN BANG SPICE IND CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using zirconocene as a catalyst has a good catalytic effect, but its price is high, and the preparation process is cumbersome, so it is not commonly used in actual production
At the present stage, in the process of preparing 2-pentylidene cyclopentanone industrially by condensation of n-valeraldehyde and cyclopentanone, the most commonly used catalysts are mostly sodium hydroxide or potassium hydroxide. Although the process is mature and the price of raw materials is relatively low, However, the process is relatively long, and after the condensation reaction, acid neutralization, sodium chloride washing, sodium carbonate washing, filtration, drying, distillation and other processes must be carried out, and there is a large amount of waste water discharge and serious pollution. Many raw material losses, low product yield, and catalysts can no longer be reused and other defects

Method used

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  • Production method of 2-pentylidene cyclopentanone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] (1) Preparation of catalyst potassium fluoride / aluminum oxide:

[0016] Dissolve 580g of potassium fluoride in 1000mL of water, add 1000g of 100-mesh granular alumina, and set the reaction temperature to 65°C, stir evenly until the reaction is over for 1 hour, then heat up and evaporate to dryness. After drying for 4 hours at an ambient temperature of about 120° C., the potassium fluoride / alumina catalyst is prepared.

[0017] (2) Condensation reaction of cyclopentanone and n-valeraldehyde: 420 g of cyclopentanone, 150 g of potassium fluoride / alumina prepared above and 1000 mL of toluene were added into a three-neck container, and the container was fixed properly. Make the stirring rod of the mechanical stirrer extend into the liquid in the three-neck container, and then connect the thermometer, the constant pressure dropping funnel and the reflux condenser to the three-neck container. Add the mixed solution of 336g of n-valeraldehyde and 1000mL of toluene into the con...

Embodiment 2

[0021] (1) Preparation of catalyst potassium fluoride / aluminum oxide:

[0022] The preparation method is as described in Example 1.

[0023] (2) Condensation reaction of cyclopentanone and n-valeraldehyde: 500 g of cyclopentanone, 150 g of potassium fluoride / alumina and 1000 mL of toluene were added to a three-neck container, and the container was fixed properly. Make the stirring rod of the mechanical stirrer extend into the liquid in the three-neck container, and then connect the thermometer, the constant pressure dropping funnel and the reflux condenser to the three-neck container. Add the mixed solution of 460g of n-valeraldehyde and 1000mL of toluene into the constant pressure dropping funnel, add the mixed solution of n-valeraldehyde and toluene dropwise while stirring, keep the reaction temperature at about 30°C, and control it within two hours After the dropwise addition was completed, the stirring was continued for one hour, and then filtered after cooling to obtain ...

Embodiment 3

[0027] (1) Preparation of catalyst potassium fluoride / aluminum oxide:

[0028] The preparation method is as described in Example 1.

[0029] (2) Condensation reaction of cyclopentanone and n-valeraldehyde: 500 g of cyclopentanone, 200 g of potassium fluoride / alumina and 1000 mL of toluene were added to a three-neck container, and the container was fixed properly. Make the stirring rod of the mechanical stirrer extend into the liquid in the three-neck container, and then connect the thermometer, the constant pressure dropping funnel and the reflux condenser to the three-neck container. Add the mixed solution of 500g of n-valeraldehyde and 1000mL of toluene into the constant pressure dropping funnel, add the mixed solution of n-valeraldehyde and toluene dropwise while stirring, keep the reaction temperature at about 30°C, and control it within two hours After the dropwise addition was completed, the stirring was continued for one hour, and then filtered after cooling to obtain ...

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Abstract

The invention provides a production method of 2-pentylidene cyclopentanone. In the method, cyclopentanone and valeraldehyde are taken as main raw material components; a used process is a condensation process; a catalyst used in a condensation reaction is potassium fluoride / alumina; after the condensation process, the method also comprises a filtering process and a post-treatment process for filtrate and a solid-phase object; the filtrate is washed with saturated solution of NaCl, dried, distilled under normal pressure and distilled under lowered pressure so as to obtain the 2-pentylidene cyclopentanone; and the solid-phase object is washed with absolute ethyl alcohol, heated and activated so as to obtain the potassium fluoride / alumina. The catalyst used in the method has high activity, iseasy for post-treatment and can be used repeatedly; the prepared 2-pentylidene cyclopentanone is fully accordant with the quality index of an intermediate product for synthesizing delta-decalactone; compared with the prior art, the method has short and simple process flow, can particularly reduce pollution caused by sewage drainage and has low cost; and the entire process is more suitable for industrialized continuous production.

Description

technical field [0001] The invention relates to a production method of fine chemical products, in particular to a production method of 2-pentylidene cyclopentanone, an intermediate of δ-decalactone series compounds. Background technique [0002] The δ-decalactone compound is an important food flavor additive. Because of its milky, coconut and fruity aroma, it is mostly used in the production process of candy, soft drink, ice cream, baked food, margarine, pastry and other foods, sometimes it is also used as a flavoring for feed, or as a daily essence and Tobacco essence and the like are widely used. The 2-pentylidene cyclopentanone referred to in the present invention is an intermediate product in the synthesis of δ-decalactone. At present, the production process of 2-pentylidene cyclopentanone mainly includes the condensation method of n-valeraldehyde and cyclopentanone, and the nucleophilic addition rearrangement method of chlorocyclopentanone and Grignard reagent. In th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/647C07C45/74
Inventor 安礼涛周建峰
Owner HUAIAN WAN BANG SPICE IND CO LTD