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Preparation technique for florosa

A lily-of-the-valley pyran and preparation process technology, applied in organic chemistry and other directions, to achieve the effects of good heat transfer and mass transfer, reduced investment in hardware equipment, and improved reaction efficiency

Inactive Publication Date: 2015-07-29
江苏绿源精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there is no report on the large-scale industrial production of pyran of lily of the valley in China. Internationally, Firmenich in Switzerland and Badische Anilin-und-Soda-Fabrik in Germany are capable of industrial production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Drop into 344.52g prenyl alcohol and 20% p-toluenesulfonic acid solution 17g (prenyl alcohol and p-toluenesulfonic acid weight ratio 1:0.05) in 1L injection reactor, drop into isovaleraldehyde 378.97g again (prenyl alcohol and p-toluenesulfonic acid The molar ratio of isovaleraldehyde is 1:1.1), and the reaction temperature is controlled at 25°C to circulate the reaction for 2 hours, and the circulation volume is controlled to 9L / h. After 2 hours, the isovaleraldehyde with a molar ratio of 1:0.005 is continuously added to the injection reactor at a rate of 35.6ml / h. Enol and 20% p-toluenesulfonic acid mixture, continuously add isovaleraldehyde with 41.4ml / h, control outward continuous discharge with 77ml / h, sampling gas chromatography detects that the lily of the valley pyran yield in the mixture is 85% , to obtain a conversion rate of 91%.

Embodiment 2

[0024] Drop into 301.45g prenyl alcohol and 20% p-toluenesulfonic acid solution 15g (prenyl alcohol and p-toluenesulfonic acid weight ratio 1:0.05) in 1L spray reactor, drop into isovaleraldehyde 452.18g again (prenyl alcohol and p-toluenesulfonic acid The molar ratio of isovaleraldehyde is 1:1.5), and the reaction temperature is controlled at 40°C to circulate the reaction for 2 hours. The circulation volume is controlled at 9L / h. After 2 hours, the isovaleraldehyde with a molar ratio of 1:0.005 is continuously added to the injection reactor at a rate of 30.5ml / h. Enol and 20% p-toluenesulfonic acid mixture, add isovaleraldehyde continuously with 48.5ml / h, control outward continuous discharge with 79ml / h, sampling gas chromatography detects that lily of the valley pyran total yield is 80% in the mixed material %, draw its conversion rate of 93%.

Embodiment 3

[0026] Drop into 344.52g prenyl alcohol and 20% p-toluenesulfonic acid solution 34.4g (prenyl alcohol and p-toluenesulfonic acid weight ratio 1:0.1) in 1L injection reactor, drop into isopentaldehyde 413.42g again (prenyl alcohol The molar ratio of isovaleraldehyde to isovaleraldehyde is 1:1.2), and the reaction temperature is controlled at 25°C to circulate the reaction for 2 hours, and the circulation volume is controlled to 9L / h. After 2 hours, control the injection reactor to continuously add isovaleraldehyde with a molar ratio of 1:0.01 at 35.5ml / h. Pentenol and 20% p-toluenesulfonic acid mixture, add isovaleraldehyde continuously with 45.2ml / h, control outward continuous discharge with 81ml / h, sampling gas chromatography detects that lily of the valley pyran total yield is in the mixed material 78%, resulting in a conversion rate of 93%.

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Abstract

The invention belongs to the technical field of fine chemical engineering, relates to florosa, and particularly relates to a preparation technique of florosa. The technical scheme provided by the invention is as follows: continuously putting isovaleraldehyde, 3-methyl-2-buten-1-ol and an acid catalyst into a jet mixing reactor for reaction according to a certain molar ratio under a certain temperature condition; meanwhile, continuously outputting reaction mixtures according to the feeding proportion so as to prepare florosa. The jet mixing reactor is used to carry out the continuous synthesis of florosa, and has better heat and mass transfer performance as compared with the conventional kettle-type batch reactor and the fixed reactor, and the reaction efficiency can be effectively improved; by adopting an acid compound as the catalyst, the conversion rate is greatly improved, the yield is up to 75-85%, and the conversion rate is up to 90% or above; meanwhile, during industrial application, by adopting the efficient jet mixing reactor, the hardware equipment investment in reaction units can be effectively reduced.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, relates to lily of the valley pyran, in particular to a preparation process of lily of the valley pyran. Background technique [0002] Lily of the valley pyran, also known as Furosa, the chemical name is 2-(2-methylpropyl)-4-methyl-4-hydropyran-4-ol, or 4-methyl-2-(2- Methylpropyl)-2H-tetrahydropyran-4-ol, its molecular structural formula is: [0003] Has a fresh, soft, natural floral aroma with notes of lily of the valley. This compound can be used in almost all types of perfumes, and can produce elegant and diffuse floral fragrance without changing the original fragrance characteristics of the essence. It is a good fragrant raw material. [0004] At present, there is no report on the large-scale industrial production of pyran of lily of the valley in China. Internationally, Firmenich in Switzerland and Badische Anilin-und-Soda-Fabrik in Germany are capable of industrial production. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D309/10
CPCC07D309/10
Inventor 范忠辉陈晓龙林广德李安
Owner 江苏绿源精细化工有限公司
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