A method for synthesizing methylheptenone by 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. It can solve the problems of product quality decline, harsh storage conditions, and complex catalyst process, and achieve the effect of reducing three wastes

Active Publication Date: 2021-03-16
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 100448830 C discloses a preparation method of a catalyst for SM reaction, the specific catalyst is hydrogenated tri(oxalato) phosphate or hydrogenated bis(oxalato) borate, and the SM reaction is used to prepare methyl Heptenone, 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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  • A method for synthesizing methylheptenone by 2-methyl-3-buten-2-ol
  • A method for synthesizing methylheptenone by 2-methyl-3-buten-2-ol
  • A method for synthesizing methylheptenone by 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 into 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 carried out for 25 minutes, and then the temperature of the reaction solution is lowered to normal temperature and pressure. The reaction liquid was distilled off under normal pressure to recover the light components 2-methoxypropene and 2,2-dimethoxypropane, and distilled under reduced pressure to obtain 167.64 g of a colorless and transparent liquid product.

[0039] Gas phase mass spectrometry was used to confirm that the resulting product was methyl heptenone, and the reaction solution was measured by gas chromatography internal standard method, and the conversion rate of raw material 2-methyl-3-buten-2-ol was 97.1%. For the product The selectivity of methyl heptenone is 98.2%, and the se...

Embodiment 2

[0041]Under normal temperature and pressure operating conditions, first 120g 2-methyl-3-buten-2-ol is added in the autoclave, pressurized and heated, so that 2-methyl-3-buten-2-ol reaches Near critical state, then, 302g of 2-methoxypropene will be pumped into the high-pressure reactor by a high-pressure liquid phase pump, and the colorless transparent liquid product 167.13g will be prepared in the same manner as in Example 1

[0042] Adopt gas phase mass spectrometry to confirm that the obtained product is methyl heptenone, and adopt the gas chromatography internal standard method identical with embodiment 1 to measure, obtain the conversion rate of raw material 2-methyl-3-buten-2-ol to be 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 changing conditions such as reaction temperature, reaction pressure, reaction time, the molar ratio of 2-methyl-3-buten-2-alcohol and 2-methoxypropene as shown in Table 1, with embodiment 1 identical Methods to obtain colorless transparent liquid products, respectively 165.63g, 164.24g, 167.59g, 162.00g, 160.26g.

[0045] Adopt gas phase mass spectrometry to confirm that the product obtained is methyl heptenone, and adopt the same gas chromatography internal standard method as Example 1 to measure the conversion rate of raw material 2-methyl-3-buten-2-ol and the conversion rate for product methyl heptenone Selectivity of heptenone 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 synthesis field of methyl heptenone, in particular to a method for synthesizing methyl heptenone 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, used for the industrial preparation of linalool, citral, ionone, vitamin A and Important intermediates such as vitamin E [Catalysis Today 121 (2007) 45-57], and also raw materials for preparing series of spices such as geraniol and nerolidol. [0003] The currently reported processes for synthesizing methylheptenone mainly include the isobutylene method, the isoprene method, the Carroll method, and the Saucy-Marbet method. [0004] Sun Yanwen and others used isobutylene, acetone and formaldehyde as raw materials to synthesize α-methylheptenone in the next step under the condition of 310-320°C and 30MPa, and then heated and converted methylheptenone under the action of pal...

Claims

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Application Information

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Patent Type & Authority Patents(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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