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Method for continuously preparing 3-methyl-2-butenol

A kind of butenol, methyl technology, applied in the preparation of medicine and pesticide intermediate 3-methyl-2-butenol, perfume field, can solve the problems of high cost, low yield, etc., to eliminate cost, raw material Easy to obtain and reduce energy consumption

Inactive Publication Date: 2012-03-07
ZHEJIANG NHU CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This route reaction classic, esterification, alkali hydrolysis yield are high, and reaction is easy to control, but the yield of isoprene and hydrogen chloride reaction is lower, about 78% (pesticide 2004,43 (5): P228-229), cause The higher cost of synthesizing 3-methyl-2-butenol

Method used

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  • Method for continuously preparing 3-methyl-2-butenol
  • Method for continuously preparing 3-methyl-2-butenol
  • Method for continuously preparing 3-methyl-2-butenol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-3

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

[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-buten-2-ol through a metering pump. Drop into 100g2-methyl-3-butene-2-alcohol earlier, vanadium oxytetraprenol ester OV(OC 5 h 9 ) 4 10.0g, start 2-methyl-3-buten-2-alcohol feeding after being warmed up to 140 ℃, 3-methyl-2-butenol crude product discharges from the side line outlet, keep reaction temperature as 140- 150°C. After finishing the feed, the crude product of 3-methyl-2-butenol was distilled off directly under reduced pressure after the reaction was completed, and combined with the output from the side line. Table 1 is the reaction result of embodiment 1-3:

[0032] Table 1

[0033] ...

Embodiment 4-6

[0034] Embodiment 4-6: Preparation of 3-methyl-2-butenol

[0035] 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-buten-2-ol through a metering pump. Drop into 100g2-methyl-3-butene-2-alcohol earlier, vanadium oxytetraprenol ester OV(OC 5 h 9 ) 4 10.0g, start 2-methyl-3-buten-2-alcohol feeding after being warmed up to 140 ℃, 3-methyl-2-butenol crude product discharges from the side line outlet, keep reaction temperature as 140- 150°C. After half of the 2-methyl-3-buten-2-ol is fed, 10.0 g of vanadium oxytetraprenol ester is added to finish the feeding. After the reaction is completed, the 3-methyl - Crude 2-butenol, combined with the side draw. Table 2 is the reaction result of embodiment 4-6:

[0036] Table 2

[0...

Embodiment 6

[0038] After the crude 3-methyl-2-butenol obtained in Example 6 was separated by rectification, 1254.1 g of 3-methyl-2-butenol was obtained, with a content of 98.2%; 2-methyl-3-butene- 2-alcohol 951.6g, content 98.5%.

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Abstract

The invention discloses a method for preparing intermediate 3-methyl-2-butenol. The prior method has the defects of rigorous conversion reaction condition, low conversion rate, difficult separation, and high technical requirement. The method has the following steps of: putting 2-methyl-3-butene-2-hydrin and rearrangement catalyst into a reaction kettle, and heating the 2-methyl-3-butene-2-hydrin and rearrangement catalyst to undergo a catalytical rearrangement reaction to obtain the mixture of the 2-methyl-3-butene-2-hydrin and the 3-methyl-2-butenol; separating the mixture through a rectification tower, recovering the 2-methyl-3-butene-2-hydrin at the top of the rectification tower and returning the 2-methyl-3-butene-2-hydrin to the reaction kettle for feeding, obtaining the crude product of the 3-methyl-2-butenol through discharging from a lateral line of the rectification tower, and continuously replenishing new 2-methyl-3-butene-2-hydrin into the reaction kettle. The method has the advantages of no use of solvent, mild reaction condition and easy control, and realizes the continuous production based on the continuous feeding and discharging.

Description

technical field [0001] The invention relates to a preparation method of spice, medicine and pesticide intermediate 3-methyl-2-butenol. Background technique [0002] 3-methyl-2-butenol, also known as isopentenol, can be used as a fragrance; 3-methyl-2-butenol derivative 3-methyl-2-butenol acetate It is also a spice and can also be used as a food additive. [0003] 3-Methyl-2-butenol is mainly used in the production of citral, isophytol (the main intermediate of VE), methyl pyritate, DV methyl chrysanthemum (intermediate of pyrethroid), synthetic vitamin A, Carotene intermediate, rubber monomer, also used in other organic synthesis. [0004] The structural formula of 3-methyl-2-butenol is as follows: [0005] [0006] At present, 3-methyl-2-butenol mainly has the following synthetic methods: [0007] (1) With 2-methyl-3-buten-2-ol as raw material, it is directly converted into 3-methyl-2-butenol under catalyst conditions. US3925485: reacted under the condition of linal...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C33/03C07C29/56
Inventor 商志才钱洪胜王金明鲁国彬邱贵生
Owner ZHEJIANG NHU CO LTD
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