Continuous preparation method of 3-methyl-2-propylene aldehyde

A kind of butenal and methyl technology, which is applied in the field of preparation of spices, medicines, and pesticide intermediates 3-methyl-2-butenal, can solve the problems of increasing separation cost and the like, and achieves reduction of operation, auxiliary, etc. of solvent recovery. The effect of less reaction and lower energy consumption

Inactive Publication Date: 2012-02-29
ZHEJIANG NHU CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This route is simple to react, but uses the highly toxic solvent o-dichlorobenzene, and increases the cost of separation

Method used

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  • Continuous preparation method of 3-methyl-2-propylene aldehyde
  • Continuous preparation method of 3-methyl-2-propylene aldehyde
  • Continuous preparation method of 3-methyl-2-propylene aldehyde

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-3

[0030] Embodiment 1-3: Preparation of 3-methyl-2-butenal

[0031] Use a kind of reaction device with the 250ml reactor of mechanical stirring, 1.5m rectifying tower, thermometer, the number of theoretical trays of rectifying tower is 30, there is a side line outlet at 10 trays from the bottom of the tower, in The feed port of the reactor realizes accurate feeding of 2-methyl-3-butyn-2-ol through a peristaltic pump. First put in 100g of 2-methyl-3-butyn-2-ol, then put in 8.0g of benzoic acid, 4.0g of titanyl acetylacetonate, and 2.0g of cuprous chloride. Alkyn-2-alcohol is fed, and the crude product of side line 3-methyl-2-butenal is discharged, keeping the reaction temperature at 120-125°C. After the feed is finished, the crude 3-methyl-2-butenal is distilled off directly under reduced pressure after the reaction is completed, and is combined with the side discharge. Table 1 is the reaction result of embodiment 1-3:

[0032] Table 1

[0033] Reaction parameters ...

Embodiment 4-6

[0035] Embodiment 4-6: Preparation of 3-methyl-2-butenal

[0036]Use a kind of reaction device with the 250ml reactor of mechanical stirring, 2.0m rectifying tower, thermometer, the theoretical tray number of rectifying tower is 40, there is side line outlet at 10 trays from the bottom of the tower, in The feed port of the reactor realizes accurate feeding of 2-methyl-3-butyn-2-ol through a peristaltic pump. First put in 100g of 2-methyl-3-butyn-2-ol, first put in 8.0g of benzoic acid, 4.0g of titanyl acetylacetonate, and 2.0g of cuprous chloride, and start 2-methyl-3- Butyn-2-ol is fed, and the crude product of side line 3-methyl-2-butenal is discharged, keeping the reaction temperature at 120-128°C. Add 8.0 g of benzoic acid, 4.0 g of titanyl acetylacetonate, and 2.0 g of cuprous chloride after feeding half of the 2-methyl-3-butyn-2-ol. The crude 3-methyl-2-butenal was distilled off and combined with the side discharge. Table 2 is the reaction result of embodiment 4-6:

...

Embodiment 6

[0039] After the crude 3-methyl-2-butenal obtained in Example 6 was separated by rectification, 1736.0 g of 3-methyl-2-butenal was obtained, with a content of 98.6%; 2-methyl-3-butyne- 2-ol 424.0g, content 98.0%.

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Abstract

The invention discloses a method for preparing an intermediate 3-methyl-2-butenoic aldehyde. The prior method uses a solvent with strong toxicity, and has rigorous reaction conditions, large separation difficulty and high cost. The method has the following steps: putting 2-methyl-3-butine-2-hydrin and a catalyst into a reaction kettle; performing a catalytical recomposition reaction through raising the temperature to obtain a mixture of the 2-methyl-3-butine-2-hydrin and the 3-methyl-2-butenoic aldehyde; separating the vaporized 2-methyl-3-butine-2-hydrin and the 3-methyl-2-butenoic aldehyde in the reaction process through a rectification tower; recovering the 2-methyl-3-butine-2-hydrin and putting the 2-methyl-3-butine-2-hydrin back into the reaction kettle for feeding; discharging materials from one side of the rectification tower to obtain the 3-methyl-2-butenoic aldehyde crude product; and replenishing new 2-methyl-3-butine-2-hydrin into the reaction kettle continuously for reaction. A solvent is not used in the method, the reaction temperature is gentle and easy to control, and the continuous production is realized by continuous feeding and discharging.

Description

technical field [0001] The invention relates to a preparation method of spice, medicine and pesticide intermediate 3-methyl-2-butenal. Background technique [0002] 3-methyl-2-butenal and its derivative 3-methyl-2-butenoic acid can be used as raw materials for fragrances. 3-Methyl-2-butenal is mainly used in the production of citral and isophytol (the main intermediate of VE), in the synthesis of vitamin A, carotenoid intermediates, rubber monomers, and in other organic synthesis. [0003] The structural formula of 3-methyl-2-butenal is as follows: [0004] [0005] At present, 3-methyl-2-butenal mainly has the following synthetic methods: [0006] (1) Use 3-methyl-2-butenol as raw material to obtain 3-methyl-2-butenal through oxidation. Chemical Communications (2007), (42), P4399-4400 adopts platinum black as a catalyst, oxidizes 3-methyl-2-butenol with hydrogen peroxide to obtain 3-methyl-2-butenal, and the yield is 91%. The disadvantage is Catalyst is expensive; Ch...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C47/21B01J31/12B01J31/02C07C45/62
Inventor 商志才钱洪胜陈洪光梁赛斌汪良标
Owner ZHEJIANG NHU CO LTD
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