Method for synthesizing 2-methylisoborneol

A technology of methyl isoborneol and mixed solution, which is applied in the field of synthesizing smell and taste substance-2-methylisoborneol, which can solve the problems of high cost, many influencing factors, and long cultivation period

Inactive Publication Date: 2009-09-16
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Because the purchase of commercial 2-methylisoborneol reagents must be imported from abroad, the cost is high; and to obtain 2-methylisoborneol...

Method used

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  • Method for synthesizing 2-methylisoborneol
  • Method for synthesizing 2-methylisoborneol
  • Method for synthesizing 2-methylisoborneol

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] The removal test of the product oxime after the reaction of embodiment 1 to camphor and hydroxylamine hydrochloride.

[0042] Because the product oxime after the reaction of camphor and hydroxylamine hydrochloride is acidic, it is diluted with distilled water and then washed with 2 mol / liter of sodium hydroxide solution, extracted twice with normal hexane, and the residual solution after extraction Figure 4c combined with n-hexane Figure 4d Carry out gas chromatographic measurement, find that greater than 98% of 2-methylisoborneol and less than 50% of oxime are in the extractant n-hexane.

Embodiment 2

[0047] In order to reduce the content of camphor in the crude product, it is necessary to find a reagent that can selectively react with camphor to generate a large number of derivatives. The resulting derivative needs to be more easily separated from 2-methylisoborneol than camphor itself. But camphor itself is inert, and many reagents are not very effective. And contriver has chosen hydroxylamine hydrochloride to react with camphor under microboiling condition, finds by gas chromatography to reaction on-line monitoring, when reaction times is 2 hours, remaining 19% camphor (see Figure 4b ); When the reaction time was 7 hours, camphor had been completely converted into the derivative of oxime (see Figure 4c ). The determination gas chromatography result of final product sees Figure 4e shown. Therefore the present invention selects 8 hours as preferred reflux reaction time.

[0048] The above crude product was separated and purified by silica gel column, with dichlorom...

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Abstract

The invention relates to a method for synthesizing a secondary metabolite of blue algae-2-methylisoborneol (the full name is 1,2,7,7-tetramethyl-outer-double ring-[2,2,1]-2-enanthol). The method comprises that d-camphor and organic compounds of magnesium (methyl magnesium iodide) are subjected to alkylation reaction to synthesize the 2-methylisoborneol, wherein the methyl magnesium iodide is prepared by the reaction of iodomethane and metal magnesium in absolute ethyl ether. The invention also relates to a method for removing impurities from the synthesized product and purifying and identifying the 2-methylisoborneol.

Description

technical field [0001] The invention relates to a method for synthesizing 2-methylisoborneol, an odor substance, and a method for qualitatively, quantitatively and purifying 2-methylisoborneol in a synthetic product. Background technique [0002] Eutrophication is the main reason for the deterioration of water quality and abnormal smell. Many eutrophic lakes have varying degrees of smell. In eutrophic water bodies, due to the excess of nutrients, the balance of the freshwater ecosystem is destroyed, which in turn causes the excessive growth of some algae biological communities. These algae and bacteria can continuously secrete and produce various secondary metabolites with odor . [0003] Smell and taste are the earliest parameters for humans to evaluate the quality of drinking water, because they can be judged intuitively by drinkers. In the past, it was believed that smell and taste had nothing to do with human health, but only limited to poor sensory properties. But n...

Claims

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Application Information

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IPC IPC(8): C07C35/29C07C29/09
Inventor 李学艳高乃云沈吉敏隋铭皓
Owner TONGJI UNIV
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