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Method for synthesis of 3-octene-2-ketone

A synthesis method and technology of octene, applied in the direction of condensation to prepare carbonyl compounds, organic chemistry, etc., can solve the problems of complex process and low product yield, and achieve the effect of high yield, less by-products and good dehydration effect

Inactive Publication Date: 2007-05-16
上海香料研究所
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The synthetic method technology of the 3-octen-2-one that adopts common way to obtain is complicated, and product yield is low

Method used

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  • Method for synthesis of 3-octene-2-ketone
  • Method for synthesis of 3-octene-2-ketone

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Experimental program
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Embodiment Construction

[0008] The implementation of the present invention will be further described below.

[0009] The first step: the preparation of 4-hydroxy-2-octanone.

[0010] Add 135g (2.33mol) of acetone, 6g (0.10mol) of acetic acid, and 2g (0.024mol) of piperidine into a 500ml round-bottomed three-necked flask equipped with a stirrer, dropping funnel, and internal thermometer. Stirring was started, and 50 g (0.58 mol) of valeraldehyde was added dropwise at about 15°C, and the addition was completed in about 1 hour, and the reaction was continued at room temperature for 3-5 hours. Stirring was stopped, and acetone was recovered under normal pressure. Distilled under reduced pressure to obtain 71 g of the product 4-hydroxy-2-octanone with a content of 95% and a yield of 85%.

[0011] The second step: the preparation of 3-octen-2-one.

[0012] Add 72g (0.5mol) of 4-hydroxyl-2-octanone, 200ml of cyclohexane, and 1g of p-toluenesulfonic acid in a 500ml round-bottomed three-necked flask equipp...

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Abstract

The invention discloses a synthesizing method of 3-octanalkylene-2-ketone, which comprises the following steps: 1. reacting acetone and valeraldehyde through condensation to prepare 4-hydroxy-2-octanone at 5-40 Deg C for 4-6h; making the molar rate of valeraldehyde and acetone at 1 / 3-1 / 5; adopting piperidine, pyrrolidone and dibutylamine as catalyst; 2. dehydrating 4-hydroxy-2-octanone through acid to prepare 3-octanalkylene-2-ketone for 0.5-1h; adopting the acid from dilute sulfuric acid, dilute hydrochloric acid, phosphoric acid and p-toluenesulfonic acid; making the solvent from cyclohexane, benzene and toluene.

Description

technical field [0001] The invention relates to a synthesis method of 3-octen-2-one. Background technique [0002] 3-Octen-2-one exists in fried hazelnuts. It has an earthy taste and a blue berry-like aroma with fruity notes. It is mainly used in soft drinks, candies, baked goods, jelly and pudding. The synthesis method of 3-octen-2-one obtained by the usual method is complex in process and low in product yield. Contents of the invention [0003] The invention aims at the shortcomings of the prior art, and provides a method for synthesizing 3-octen-2-one with higher yield. [0004] The synthetic method of 3-octene-2-one of the present invention: the first step, make 4-hydroxyl-2-octanone by condensation reaction with acetone and valeraldehyde, reaction temperature 5-40 ℃, reaction time 4-6 hour, the molar ratio of valeraldehyde to acetone is 1 / 3 to 1 / 5, and the catalyst used in the reaction is piperidine, pyrrolidine, dibutylamine; in the second step, 4-hydroxyl-2-octano...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/45C07C49/203
Inventor 章平毅吴越芳
Owner 上海香料研究所
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