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Synthetic method for epoxy sclareol

A synthesis method and technology of sclareol, applied in the direction of organic chemistry and the like, can solve the problems of high cost, low atom utilization rate, poor stability of peroxyacid, etc., and achieve the effect of low product cost

Inactive Publication Date: 2005-10-19
SHAANXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the obvious disadvantages of peracid as oxidizing agent are high cost, low atomic utilization rate, and relatively long reaction time.
In addition, many peroxyacids have poor stability, are easy to decompose during transportation, storage and use, and sometimes explode, and their safety is poor

Method used

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  • Synthetic method for epoxy sclareol
  • Synthetic method for epoxy sclareol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Dissolve 30.8g of sclareol in 90mL of 1,2-dichloroethane, add 1.5g of 12-phosphotungstic acid, 0.72g of cetylpyridinium chloride and 35mL of 30% aqueous hydrogen peroxide to adjust the pH to ≈2.0 , stirred vigorously at 70°C for 12 hours. The obtained reaction mixture was separated and purified according to conventional methods to obtain 30.4 g of epoxy sclareol as a white solid, with a yield of 93.8%. The melting point is 131-132°C.

Embodiment 2

[0028] Dissolve 30.8g of sclareol in 60mL of chloroform, and add 0.41g of sodium tungstate dihydrate, 0.72g of sodium dihydrogen phosphate, 0.36g of cetylpyridinium chloride and 90mL of 10% hydrogen peroxide solution to adjust the pH to ≈1.5 , stirred vigorously at 70°C for 24 hours. The resulting reaction mixture was separated and purified by conventional methods to obtain 28.4 g of epoxy sclareol as a white solid, with a yield of 87.8%. The melting point is 130-132°C.

Embodiment 3

[0030] Dissolve 30.8g of sclareol in 60mL of ethyl acetate, add 2.0g of hexadecyl phosphotungstate pyridinium salt and 21mL of 50% hydrogen peroxide aqueous solution, and react vigorously at 70°C for 8 hours. The resulting reaction mixture was separated and purified by conventional methods to obtain 30.2 g of epoxyslareol as a white solid, with a yield of 93.2%. The melting point is 130-132°C.

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Abstract

The epoxy sclareol is synthesized with sclareol as main material, hydrogen peroxide solution as oxidant, and water and / or organic solution of transition elements, especially VB or VIB transition elements as the catalyst for activating hydrogen peroxide. Inside the homogeneous or two-phase water-organic solvent system, there is also of kind of phase transfer catalyst, so as to epoxidize sclareol into epoxy sclareol and to obtain epoxy sclareol through conventional separation and purification. Compared with available technology, the present invention uses cheap and clean hydrogen peroxide aqua as oxidant and has the advantages of simplicity, cleanness, high efficiency, high safety and low cost.

Description

technical field [0001] The invention relates to a synthesis method of epoxy compounds, in particular to a synthesis method of epoxy sclareol. Background technique [0002] Epoxyslareol is a synthetic fragrance Ambrox [chemical name 1, 2, 3a , 4,5,5a,6,7,8,9,9a,9b-decahydro-3a,6,6,9a-tetramethylnaphtho[2,1-b]furan, trade name Ambrox, Ambroxan, Amberoxide, etc.] and sclareolide [chemically known as 1,2,3a,4,5,5a,6,7,8,9,9a,9b-dodecahydro-3a,6,6,9a-tetramethyl An important intermediate of naphtho[2,1-b]furan-2(1H)-one]. Epoxy sclareol is also an important raw material for the preparation of sclareol [chemical name 8α, 13, 14, 15-tetrahydroxy raberdan]. [0003] In the previously reported method, epoxy sclareol is synthesized by epoxidizing sclareol with organic peroxyacid as oxidant. The synthesis method disclosed in German patent (DE4 124 726) is to carry out epoxidation reaction of sclareol with m-chloroperbenzoic acid (m-CPBA) in the presence of sodium acetate in an orga...

Claims

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Application Information

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IPC IPC(8): C07D303/14
Inventor 魏俊发吴亚石先莹张勇民
Owner SHAANXI NORMAL UNIV
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