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The preparation method of 3-methyl-3-penten-2-one

A technology of pentene and methyl is applied in the field of preparation of intermediate 3-methyl-3-penten-2-one, can solve the problems of high production cost, serious environmental pollution and high equipment requirements, and achieves energy consumption and Low production cost, high yield and purity, and the effect of reducing separation difficulty

Active Publication Date: 2016-03-02
NANJING ENETEKS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The above methods all adopt strong acid or strong base as the conditions for the condensation of methyl ethyl ketone and acetaldehyde, which has high production cost, serious environmental pollution, and high requirements for equipment. Therefore, it is necessary to invent more environmentally friendly, lower energy consumption and lower production costs. , 3-methyl-3-penten-2-one preparation method with stronger industrial reliability to meet the needs of ambroxone production

Method used

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  • The preparation method of 3-methyl-3-penten-2-one

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Under normal pressure, add 540g methyl ethyl ketone (AR) and 162g American Rohm and Haas dry hydrogen Amberlyst15 catalyst to a 1L glass stirred tank reactor, store 165g acetaldehyde (99%) in the dropping funnel, drop the dropping funnel The lower port is provided with a catheter extending into the bottom of the reactor, and the reaction is heated by a water bath. When the temperature reaches 45°C, acetaldehyde is added dropwise to the reactor, and the dropwise time of acetaldehyde is controlled to be 1.5h, and the reaction is continued after the drop is completed. After 3 hours, the reaction was stopped, and the material obtained after the reaction was analyzed by chromatography. It was determined that the single-pass conversion rate of butanone was 48%, the selectivity of 3-methyl-3-penten-2-one was 92%, and some impurities were generated in the rest.

[0021] The material obtained after the reaction enters the separation unit, distills and recovers butanone and separa...

Embodiment 2

[0023] Under normal pressure, add 540g methyl ethyl ketone (AR) and 162g American Rohm and Haas dry hydrogen Amberlyst35 catalyst to a 1L glass stirred tank reactor, store 275g acetaldehyde (99%) in the dropping funnel, drop the dropping funnel The lower port is provided with a catheter extending into the bottom of the reactor, and the reaction is heated by a water bath. When the temperature reaches 55°C, acetaldehyde is added dropwise to the reactor. The time for adding acetaldehyde is controlled to be 1h, and the reaction is continued for 1h after the drop is completed. Afterwards, the reaction was stopped, and the material obtained after the reaction was analyzed by chromatography to determine that the single-pass conversion rate of butanone was 67%, the selectivity of 3-methyl-3-penten-2-one was 96%, and the rest generated some impurities.

[0024] The material obtained after the reaction enters the separation unit, distills and recovers butanone and separates impurities, a...

Embodiment 3

[0026] In a 5L double-layer glass stirred reactor, add 1800g butanone and 900g LANXESS dry-type LewatitK2620 catalyst, store 1100g of acetaldehyde (99%) in the liquid storage tank, and the double-layer glass stirred reaction passes through the interlayer. Enter hot water for heating, when the temperature reaches 50°C, use a peristaltic pump to input acetaldehyde at a constant speed to the bottom of the reactor, control the input time of acetaldehyde to 2h, then continue to react for 0.5h and then stop the reaction, and analyze the obtained product by chromatography As for the material, it is determined that the single-pass conversion rate of butanone is 82%, the selectivity of 3-methyl-3-penten-2-one is 93%, and the rest generate some impurities.

[0027] The material obtained after the reaction enters the separation unit, distills and recovers butanone and separates impurities, and the purity of 3-methyl-3-penten-2-one obtained after separation is 97.7%.

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Abstract

The invention relates to a preparation method of 3-methyl-3-amylene-2-ketone. The preparation method comprises the steps of mixing butanone and a solid acid catalyst at 0-80 DEG C, adding acetaldehyde, fully mixing, reacting continuously, separating and purifying after reaction to obtain the 3-methyl-3-amylene-2-ketone, wherein the solid acid catalyst is highly-acidic dry type sulfonic acid group based polystyrene with H<+> or sulfonic acid group based perfluorination cation exchange resin. According to the method, the solid acid catalyst is adopted, compared with the traditional synthetic method that strong acid and strong base are used, the method can greatly reduce the follow-up separation difficulty and environment pollution degree, no equipment corrosion is caused, and the product yield and the purity are high, therefore, the preparation method of 3-methyl-3-amylene-2-ketone is green and environment-friendly; and besides, no assisted solvent is adopted, the follow-up separation difficulty is reduced, the energy consumption and the production cost are low, and the industrial reliability is strong.

Description

field of invention [0001] The invention relates to the field of perfumes, in particular to a preparation method for an intermediate 3-methyl-3-penten-2-one used for synthesizing ambroxone. Background technique [0002] The route of synthetic ambroxone mainly contains three steps at present: 1, synthesis 3-methyl-3-penten-2-one, 2, myrcene and 3-methyl-3-penten-2-one carry out diene addition 3, the cyclization of the diene addition product, and when the first step synthesizes 3-methyl-3-penten-2-one, the following methods are mainly used: [0003] Huang Rongchu et al. (Guangzhou Chemistry, 1990) slowly added acetaldehyde dropwise to the mixed solution of butanone, potassium hydroxide and methanol at low temperature. After stirring for 1 hour, oxalic acid was added to form calcium oxalate, then filtered, and then the butanone was removed. and impurities to obtain yellow transparent 3-methyl-3-penten-2-one; [0004] Chinese patent CN101081808A discloses a method for synthesiz...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/203C07C45/74
CPCC07C45/74C07C49/203
Inventor 杨高东林力克周政王宝荣张志炳
Owner NANJING ENETEKS
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