Method for synthesizing methyl heptenone from 2-methyl-3-buten-2-ol

A technology for synthesizing methylheptenone and alcohol, which is applied in the direction of condensation to prepare carbonyl compounds, organic chemistry, etc., can solve the problems of product quality decline, easy deterioration, harsh storage conditions, etc., and achieve the effect of reducing three wastes

Active Publication Date: 2018-07-20
ZHEJIANG NHU CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This catalyst has a high reaction yield, but the halogen contained in the catalyst corrodes the equipment greatly, and in the production and separation process, there will be halogen in the entire reaction and separation system, resulting in a decline in product quality and a substantial increase in equipment investment
[0012] CN 100448830C discloses a kind of preparation method of the catalyst that is used for SM reaction, and concrete catalyst is hydrogenated tri(oxalato) phosphate or hydrogenated bis(oxalato) borate, carries out SM reaction with this catalyst and prepares methylheptyl Enone, the highest selectivity can reach 97%, and the yield can reach 95%, but the preparation process of the catalyst is complicated, and the storage conditions are harsh, and it is easy to deteriorate
[0013] Through the modification of phosphoric acid, the yield has been greatly improved, but there is still a considerable amount of by-product isoprene, how to avoid the formation of isoprene, the method provided in this paper can solve this problem

Method used

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  • Method for synthesizing methyl heptenone from 2-methyl-3-buten-2-ol
  • Method for synthesizing methyl heptenone from 2-methyl-3-buten-2-ol
  • Method for synthesizing methyl heptenone from 2-methyl-3-buten-2-ol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Under normal temperature and pressure operating conditions, first add 120g of 2-methyl-3-buten-2-ol and 302g of 2-methoxypropene to the autoclave, pressurize to 6MPa, and heat to 260°C, When the near-critical state of 2-methyl-3-buten-2-ol is reached, the Saucy-Marbet reaction is performed for 25 minutes, and then the temperature of the reaction liquid is lowered to normal temperature and pressure. The reaction liquid was distilled under normal pressure to remove and recover the light components of 2-methoxypropene and 2,2-dimethoxypropane, and distill under reduced pressure to obtain 167.64 g of a colorless and transparent liquid product.

[0039] The product obtained was confirmed to be methyl heptenone by gas mass spectrometry. The reaction liquid was measured by gas chromatography internal standard method, and the conversion rate of the raw material 2-methyl-3-buten-2-ol was 97.1%. The selectivity of methylheptenone is 98.2%, and the selectivity to by-product isoprene ...

Embodiment 2

[0041] Under normal temperature and pressure operating conditions, first add 120g of 2-methyl-3-buten-2-ol to the autoclave, pressurize and heat it to make 2-methyl-3-buten-2-ol reach Near the critical state, then, 302 g of 2-methoxypropylene was pumped into the autoclave by a high pressure liquid phase pump, and 167.13 g of a colorless and transparent liquid product was prepared in the same manner as in Example 1.

[0042] The product was confirmed to be methylheptenone by gas mass spectrometry, and the same gas chromatography internal standard method as in Example 1 was used for measurement. The conversion rate of the raw material 2-methyl-3-buten-2-ol was 98.1%. , The selectivity to the product methylheptenone was 96.9%, and the selectivity to the by-product isoprene was 0.064%. The measurement results are shown in Table 1.

Embodiment 3-7

[0044] Except for changing the reaction temperature, reaction pressure, reaction time, and the molar ratio of 2-methyl-3-buten-2-ol to 2-methoxypropene as shown in Table 1, the same as in Example 1 The method obtains colorless and transparent liquid products, which are respectively 165.63g, 164.24g, 167.59g, 162.00g, and 160.26g.

[0045] The obtained product was confirmed to be methylheptenone by gas mass spectrometry, and the same gas chromatography internal standard method as in Example 1 was used for measurement to obtain the conversion rate of the raw material 2-methyl-3-buten-2-ol and the product The selectivity of ylheptenone and by-product isoprene. The measurement results are shown in Table 1.

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Abstract

The invention relates to a method for synthesizing methyl heptenone from 2-methyl-3-buten-2-ol. 2-methyl-3-butene-2-alcohol takes Saucy-Marbet reaction with 2-alkoxylpropylene in the near critical state to obtain methyl heptenone. The synthesis method has the advantages that the use of catalysts is not needed; the selectivity of the product of methyl heptenone can be improved.

Description

Technical field [0001] The invention relates to the field of synthesis of methylheptenone, in particular to a method for synthesizing methylheptenone from 2-methyl-3-buten-2-ol. Background technique [0002] Methylheptenone, chemical name: 6-methyl-5-hepten-2-one, is an important fine chemical intermediate for the industrial preparation of linalool, citral, ionone, vitamin A and Important intermediates such as vitamin E [Catalysis Today121(2007)45-57] are also raw materials for the preparation of geraniol, nerolidol and other spices. [0003] The currently reported processes for synthesizing methylheptenone mainly include isobutylene method, isoprene method, Carroll method, and Saucy-Marbet method. [0004] Sun Yanwen et al. used isobutylene, acetone and formaldehyde as raw materials to synthesize α-methylheptenone in the next step at 310-320℃, 30MPa, and then heated and converted to methylheptenone under the action of palladium and carbonyl iron catalyst. This reaction When prepar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/45C07C49/203
CPCC07C45/45C07C49/203
Inventor 王旭明王钰白发明文顺利邵闪
Owner ZHEJIANG NHU CO LTD
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