Method for separation purification of sclareolide from synthetic sclareol composites

A technology of sclareolide and sclareolide, which is applied in the direction of organic chemistry and the like, can solve the problems of complex process, long operation time, large solvent consumption and the like, and achieves the effects of high yield, short operation time and simple process

Inactive Publication Date: 2005-03-16
TIANJIN UNIV
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

Although the above-mentioned method can obtain the sclareolide of required purity, in this process, an extractant is added, so that the final product contains residual solvent, which greatly limits the application of sclareolide as a medicine and food flavoring agent; In addition, this method has complex process, long operation time, and consumes a large amount of solvent

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment Construction

[0006] Add 200g of sclareolactone block solid mixture to the feeder of molecular distillation device (feeder volume 250ml, evaporation area 4.8 square decimeters, wiper speed 50~1000rpm), containing 90.5% of sclareolide %. Turn on the raw material preheating device, raise the temperature to 97°C, dissolve the solid and maintain a constant temperature. Turn on the cooling device, keep the cooling temperature at 35°C, add liquid nitrogen into the cold trap, turn on the rotary vane vacuum pump to make the operating pressure of the system reach 1.5Pa, turn on the precision constant temperature tank for evaporating materials to heat the heat transfer oil, so that the temperature Stabilize at the desired evaporation temperature of 99°C, then start the feed valve, the feed rate is 100g / h, and the rotating speed of the wiper is 138rpm. After the distillation process ends, 18.5g of distillate and 181.5g of heavy fraction are obtained; The heavy distillate obtained from the first disti...

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Abstract

The invention provides a method for separation purification of sclareolide from synthetic sclareol composites by using molecular distillation device for operation under pressure of 0.01-100.0Mpa, evaporative temperature 50-200 deg. C, cool-down temperature -15-80 deg. C, temperature difference between the evaporator and condenser 30-215 deg. C, the agitating speed 10-1000 rp.

Description

technical field [0001] The invention relates to a method for separating and purifying sclareolactone from a reaction compound of sclareol, which belongs to the deep processing and utilization technology of sclareol. Background technique [0002] Sclareolide is generally synthesized by reaction of sclareol, and CN92104935 reports a method for extracting sclareol from the residue of Sclareol. Patents such as US5247100, US5212078, WO2004013069, JP2002371031, JP2001247561 and US5525728 have reported the synthesis method of sclareolide: dissolve sclareol with organic solvent, then add alkaline substance, hypochlorite, ruthenium catalyst and phase transfer catalyst , after one step of oxidation and heating, sclareolactone can be obtained. Patents such as US5906993, US5372834, US4999207, US4988532, US4960603, US4917913, US20030072777 (A1), WO03007734 and US6331551 have reported the efficacy of high-purity sclareolide: for the treatment of infectious diseases caused by microorganis...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/92
Inventor 许松林应安国王淑华向爱双徐世民
Owner TIANJIN UNIV
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