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Method for preparing sclaveol by sclaveol concrete

A technology of sclareol and extract, applied in the field of preparation of sclareol, capable of solving the problems of low purity and cumbersome operation steps

Inactive Publication Date: 2008-07-30
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Taking a comprehensive view of the existing methods for preparing sclareol from sclareol extract, the disadvantages of its existence are that the operating steps are cumbersome and the purity of the product (slareol) is not high (generally 80wt%~90wt%)

Method used

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preparation example Construction

[0012] The said method of preparing sclareol of the present invention, comprises the steps:

[0013] 1, Sclareol extract (the content of Sclareol is greater than 45wt%) and C 6 ~C 9 Saturated alkanes are placed in a reactor, and then sodium hydroxide, potassium hydroxide or calcium hydroxide are added into the reactor in an amount of 5% to 20% of the weight of the sclareol extract. After reacting at ℃ for 1-5 hours, let it stand still, and divide off the water phase to obtain the organic phase.

[0014] 2. Under the condition of 30°C-70°C, wash the organic phase obtained in step 1 with a phosphate or acetate buffer solution with a pH value of 5.0-8.0 until the color of the aqueous phase does not change after washing (pH value is 7.5 ~11), while the organic phase is clear and transparent, the purpose of washing is to remove some saponification products and some pigments present in the organic phase. The organic phase is crystallized at -10°C to 0°C, and the crystal is obtain...

Embodiment 1

[0018] Dissolve 40g of Sclareus extractum (about 45wt% of sclareol content) in 240ml of n-heptane, add 100ml of aqueous sodium hydroxide solution with a concentration of 5wt% to saponify after completely dissolving, and saponify at 90°C for 2 hours , stand still, separate the water phase, take the upper alkane phase, add 60ml of acetate buffer solution with a temperature of 45°C, wash, let stand, separate the water phase, wash three times, and store the washed organic phase at -3 Freeze and crystallize at ℃, filter after 12 hours, and vacuum-dry the sclareol crystals at 50°C to obtain 15.72 g of sclareol finished product, the content of sclareol is 94.21wt%.

Embodiment 2

[0020] Dissolve 40g of Sclareus extract (about 45wt% of sclareol content) in 180ml of n-octane, and after completely dissolving, add 60ml of potassium hydroxide aqueous solution with a concentration of 10wt% for saponification, and saponify at 95°C for 1.5 hours , stand still, separate the water phase, take the upper alkane phase, add 40ml of phosphate buffer solution with a temperature of 55°C to wash, let it stand, separate the water phase, wash twice, and put the washed alkane phase at -5 Freeze and crystallize at ℃, filter after 12 hours, and vacuum-dry the sclareol crystals at 50°C to obtain 15.24 g of finished sclareol, the sclareol content is 95.76 wt%.

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Abstract

The invention relates to a method for preparing fragrant perilla alcohol by using a fragrant perilla alcohol extract. The invention principally relates to the following steps: the fragrant perilla alcohol extract is placed into an organic solvent; saponification is carried out under the condition of temperature of 50 to 130 DEG C and no existing inorganic base. The obtained organic phase is washed by the buffer solution with a pH value of 5.0 to 8.0 and is then crystallized under the temperature of minus 20 to 0 DEG C for obtaining the target product. Compared with the present method of preparing the fragrant perilla alcohol by using the fragrant perilla alcohol extract, the invention has the advantages that the preparation process is simple and is friendly with the environment (the solvent used in the preparation process can all be recycled and reused), and the obtained product has a high purity (the content of the fragrant perilla alcohol is more than 93 wt percent).

Description

technical field [0001] The invention relates to a method for preparing sclareol, in particular to a method for preparing sclareol from a sclareol extract. Background technique [0002] Sclareol (also known as stearyl alcohol, which belongs to diterpene alcohols), is a natural plant fragrance, which is mainly used in the preparation of daily essence and preparation of ambergris (a kind of precious fragrance). In addition, because sclareol has biological activity, it also has certain medical and agricultural value. [0003] Enriched from the sclareol extract (the residue of the inflorescence of Sclareus after oil extraction, then leached and concentrated with petroleum ether, the content of sclareol is 40wt%-50wt%) Sclareol is one of many methods for preparing sclareol. As reported in US.Pat.No.3,060,172: first adopt solvent extraction sclareol extract, then use ethanol aqueous solution to extract gained extract, finally concentrate the extract of gained, obtain the extract ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C35/36C07C29/74
Inventor 陈葵洪海纪利俊武斌朱家文
Owner EAST CHINA UNIV OF SCI & TECH
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