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Method for producing methyl heptenone

A technology of methyl heptenone and methyl butenol, which is applied in the field of synthesis of methyl heptenone, can solve the problems such as the inability to increase the yield, and achieve the effect of increasing the yield and reducing the production cost

Inactive Publication Date: 2012-06-20
中天科盛科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the preparation process of methyl heptenone, due to the heat sensitivity of methyl heptenone, the methyl heptenone produced by the reaction will be partially cracked into isoprene and acetone when the temperature is 148-151 ° C. Pentadiene continues to undergo oligomerization to form heavy components, so that the yield of the reaction cannot be increased

Method used

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  • Method for producing methyl heptenone
  • Method for producing methyl heptenone
  • Method for producing methyl heptenone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～10

[0019] The reaction is carried out in a reactive distillation device, which is composed of a reactor and a rectification column. The reactor is a 1000ml glass reactor with a three-neck flask. The left and right sides are respectively the raw material inlet and the temperature measuring thermometer socket. The middle top is connected to the rectification column. The theoretical plate number of the rectification column is 18. Condensation and reflux devices at the vent and outlet.

[0020] First add 100 grams of methyl heptenone and an appropriate amount of catalyst into the reactor, heat the reactor to 140-160 ° C, and then maintain the temperature to continuously pump the prepared methyl butenol and methyl acetoacetate solution into the reaction The device reacts. The reaction pressure is normal pressure, and the reflux ratio of rectification is controlled. The carbon dioxide produced by the reaction is discharged through the vent at the top of the rectification column, and ...

Embodiment 11

[0029] A method for producing methyl heptenone, the raw material methyl butenol and methyl acetoacetate are placed in a reactor, the molar ratio of methyl butenol and methyl acetoacetate is 1.1:1, and the reaction temperature is 140°C , the reaction time is 5 hours, the catalyst that adopts is aluminum isopropoxide / diethanolamine composite catalyst, wherein the consumption of aluminum isopropoxide catalyst is 1% of the methyl acetoacetate feeding quality, the mol ratio of diethanolamine / aluminum isopropoxide The ratio is 0.1:1, and high-purity methyl heptenone is prepared by catalytic transesterification and Caroll reaction.

Embodiment 12

[0031] A method for producing methyl heptenone, the raw material methyl butenol and methyl acetoacetate are placed in a reactor, the molar ratio of methyl butenol and methyl acetoacetate is 1.2:1, and the reaction temperature is 146°C , the reaction time is 8 hours, the catalyst that adopts is aluminum isopropoxide / diethanolamine composite catalyst, wherein the consumption of aluminum isopropoxide catalyst is 2% of the methyl acetoacetate feeding quality, the mol ratio of diethanolamine / aluminum isopropoxide The ratio is 0.2:1, and high-purity methyl heptenone is prepared by catalytic transesterification and Caroll reaction.

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Abstract

The invention relates to a method for producing methyl heptenone. In the method, high-purity methyl heptenone is prepared by performing catalytic ester exchange and a Caroll reaction on methyl butenol and methyl acetoacetate in the molar ratio of (1.1-2.0):1; a catalytic reaction temperature is 140-160 DEG C; reaction time is 5-12 hours; an aluminum isopropoxide / diethanol amine compound agent is adopted; the using amount of the aluminum isopropoxide is 1-4 percent of the inventory rating of the methyl acetoacetate; and the molar ratio of diethanol amine to the aluminum isopropoxide is (0.1-0.5):1. Compared with the prior art, the method has the advantages that: an appropriate compound catalyst is selected, and the cracking reaction rate of the methyl heptenone during the reaction is suppressed, so that the reaction yield is remarkably increased, and production cost is greatly lowered.

Description

technical field [0001] The present invention relates to the synthesis method of methyl heptenone, in particular to a composite catalyst made of aluminum isopropoxide and diethanolamine using 2-methyl-3-buten-2-ol and methyl acetoacetate as raw materials The method for preparing methyl heptenone under action. Background technique [0002] Methylheptenone is a colorless or pale yellow liquid with a lemongrass and isobutyl acetate-like aroma. It has a strong chemical reaction ability and can be used as an important intermediate in the synthesis of various medicines, flavors and fragrances. Methylheptenone is the main raw material for the preparation of linalool, citral and pseudoionone, which can be further used to prepare vitamin A, vitamin E, vitamin K1 and various flavors and fragrances. [0003] At present, the preparation of methyl heptenone mainly takes 2-methyl-3-buten-2-ol (methylbutenol) and methyl acetoacetate as raw materials, under the action of aluminum isopropox...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/203C07C45/68B01J31/22
Inventor 陈盛
Owner 中天科盛科技股份有限公司
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